Sciencemadness Discussion Board

Make Potassium (from versuchschemie.de)

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AndersHoveland - 7-2-2012 at 14:49

I have been thinking about the possibility of reducing sodium hydroxide with aluminum foil. So a calculation of the expected enthalpy of formation of such a reaction may be helpful, to get some idea as to whether such a reaction would be expected to be favorable.

The enthalpy of formation for Al2O3 is -1669.8 kJ/mol, while the value for Na2O is -414.2 kJ/mol.

As Al2O3 contains 3 times as many oxygen atoms per mol, 3 times 414.2 equals 1242.6, which is still less than 1669.8, so aluminum has more affinity for oxygen than sodium. And indeed an exothermic thermite reaction between sodium hydroxide and aluminum powder can produce sodium.
http://www.youtube.com/watch?v=908rjHQ5mmc

The enthalpy of formation for AlCl3 is -705.63 kJ/mol, while the value for NaCl is -411.12 kJ/mol.

As 3 times 411.12 equals 1233.36, sodium has more affinity for chlorine than aluminum. And indeed, the reduction of aluminum chloride by elemental sodium was first done by H. Sainte-Claire Deville, although H. C. Ørsted had previously used potassium instead.


But of course the interaction with the alcohol would affect the enthalpy of formation, increasing the affinity of sodium for oxygen. A quick estimation of this effect can be made by comparing the enthalpy of formation for sodium hydroxide, which is no doubt even more favorable than sodium alkoxides (sodium alkoxides vigorously hydrolyse with water).

NaOH -425.93 kJ/mol
H2O -285.83 kJ/mol
Na2O is -414.2 kJ/mol

So the hydration of sodium oxide to anhydrous sodium hydroxide should release 151.83 kJ for each mole of Na2O reacted.
Na2O + H2O --> 2 NaOH

So it can be inferred that the presence of tert-butanol would not significantly affect the affinity of sodium for oxygen, meaning that the reduction of a sodium alkoxide by aluminum should still be energetically favorable.


The competing affinities between sodium and aluminum for fluorine apparently is more complicated:
Quote:

It will be noted that when aluminum fluoride is in excess to that contained in cryolite (NaF)6Al2F6, aluminum does not reduce sodium fluoride, and on the other hand, when sodium fluoride is in excess, aluminum does reduce sodium fluoride.
Metallurgical and Chemical engineering, Volume 11, p178 (1913)

condennnsa - 7-2-2012 at 22:37

Well aluminum powder does reduce NaOH. But only to NaH I think. This was discussed in the unconventional sodium thread I think. I have tried it myself. ground up equal amounts of NaOH and Al powder , and started heating it with a torch. First it starts bubbling a lot of hydrogen gas, but this is not the reaction, if you heat the pile to red-orange heat, at some point a thermite-like reaction occurs, and the whole thing gets white hot. IRC some people successfully isolated potassium with this approach, but not sodium. After my pile cooled down i broke it up and could not see any shiny metal, when i put it water it reacted releasing a lot of hydrogen , but not like sodium, not violent. So I concluded that aluminum is oxidised to Al2O3, and what's left behind is mostly sodium hydride which reacted with water.

[Edited on 8-2-2012 by condennnsa]

AndersHoveland - 7-2-2012 at 23:28

That could be possible. KH is apparently a more reactive reducing agent than NaH. NaH is also more stable, decomposing to its elements at a much higher temperature than KH. NaH begins to decompose at 330°, KH at 200°. ( O. Ruff ) Wikipedia gives much higher values at around 800° and 400°, respectively.
Quote:

Pyrrolidone is completely metallated in 2-3 hr at room temperature with KH, while no reaction is observed with either a potassium dispersion or NaH. At elevated temperatures (above 75 C), both K and NaH react, slowly liberating hydrogen, however, at 75 C the amide evidently undergoes secondary decompositions as fast as formed for the solutions never develop sufficient base strength to deprotonate triphenylmethane indicator detectably.

The solvents which appear most suitable for reactions with KH are ethers. Aromatic hydrocarbons are inert to KH.


"Potassium hydride, highly active new hydride reagent"
Charles Allan Brown
J. Org. Chem., 1974, 39 (26), pp 3913–3918




However, an alternate explanation for why potassium was isolatable from the thermite mixture is that, at such high temperatures, it is significantly more volatile (lower boiling point).

I do not know whether potential formation of NaH is possible in a liquid tert-butanol reaction using NaOH, since NaH reacts with alcohols to form sodium alkoxides and H2.

Also, I found something which might possibly explain why only sterically hindered alcohols, such as tert-butanol, seem to work in the reaction.
Quote:

NaH has been successful only in reactions involving relatively acidic compounds (e.g. ethyl acetoacetate, unhindered alcohols )


[Edited on 8-2-2012 by AndersHoveland]

blogfast25 - 8-2-2012 at 06:50

Quote: Originally posted by AndersHoveland  
I have been thinking about the possibility of reducing sodium hydroxide with aluminum foil. So a calculation of the expected enthalpy of formation of such a reaction may be helpful, to get some idea as to whether such a reaction would be expected to be favorable.



It’s already been done, on this forum. It creates a mess, from which the sodium is practically irrecoverable.

To apply it as on this thread would require Al butoxide to form and be sufficiently stable.

Look at NaF + Al:

NaF: STP HoF = - 577 kJ/mol (Wolfram Alpha)
AlF3: STP HoF = - 1423 kJ/mol (NIST Webbook)

NaF + 1/3 Al == > Na + 1/3 AlF3: STP HoR = 577 + 1/3 x (- 1423) = + 102 kJ/mol

But: AlF3 MP = 1291 C, Na BP = 883 C. By heating a mixture of NaF and Al to about 1000 C in vacuum it may be possible to distil off sodium vapour, 'pulling'. the equilibrium to the right... I, for one, will not be trying this. ;)

I will 'shortly' (it's bitterly cold here) try dihydro myrcenol (a tertiary alcohol with longer chain length) for K synth.

[Edited on 8-2-2012 by blogfast25]

TheChemINC - 23-2-2012 at 17:24

I didnt understant the german version of this but i know that you can heat magnesium and potassium hydroxide in mineral oil while it is refluxing. Then if you add a tertairy alcohol, like T-butanol for instance.... it will catalyse the reaction and help coalesce the potassium metal that is formed..... check out a video by a guy named NurdRage on youtube.... most of you guys have probably heard of him, but he gives an excellent explanation of the process. also, not to change the subject, but does anyone know where i could get or how to make t-butanol?

bfesser - 23-2-2012 at 17:43

If you had bothered to read the thread, you'd find that everything you've just stated had been discussed already. NurdRage even participated in the discussion, if I remember correctly. As for t-butanol, refer to your cross-post--and use the search function next time. You'll find that most members don't take too kindly to strangers who don't know how to use Google or the forum search function. ;)

TheChemINC - 24-2-2012 at 03:30

oh, sorry. didnt mean to piss andyone off..... :/

White Yeti - 24-2-2012 at 12:32

Quote: Originally posted by TheChemINC  
oh, sorry. didnt mean to piss andyone off..... :/


Don't sweat it, we're just pointing you in the right direction. Many long time members are rough on beginners.

Welcome to the forum!

TheChemINC - 24-2-2012 at 15:20

thanks...... i was just trying to figure this out :P

Waffles SS - 24-2-2012 at 22:36

I didnt read all of this 37 pages( i just read 10 or less pages) but i am interest to know : does this method is usable for making lithium metal?

White Yeti - 25-2-2012 at 06:18

Quote: Originally posted by Waffles SS  
I didnt read all of this 37 pages( i just read 10 or less pages) but i am interest to know : does this method is usable for making lithium metal?


It should be, but considering it doesn't yet work with sodium, it would be quite a stretch. Besides, you can get lithium from batteries. This is not the case with sodium or potassium metal.

TheChemINC - 25-2-2012 at 09:26

you can use lithium as a reducing agent to make potassium or sodium though.....

i took lithium foil from a battery and poured potassium chloride over it. after i heated it up with a bunsen burner, i place a watchglass over the top of the test tube i used. then i broke apart the test tube and threw the material that formed in the bottom into a beaker of water and purple flames appeared instantly. it was pretty cool.... im not sure that it is efficient and the product is very crude and mixed with tons of other crap.....

blogfast25 - 25-2-2012 at 10:26

Quote: Originally posted by Waffles SS  
I didnt read all of this 37 pages( i just read 10 or less pages) but i am interest to know : does this method is usable for making lithium metal?


The patent specifies Na (but to do harder than K), K and Cs. Definitely not Li.

blogfast25 - 25-2-2012 at 10:34

Quote: Originally posted by TheChemINC  
you can use lithium as a reducing agent to make potassium or sodium though.....

i took lithium foil from a battery and poured potassium chloride over it. after i heated it up with a bunsen burner, i place a watchglass over the top of the test tube i used. then i broke apart the test tube and threw the material that formed in the bottom into a beaker of water and purple flames appeared instantly. it was pretty cool.... im not sure that it is efficient and the product is very crude and mixed with tons of other crap.....


It's not efficient at all that way. Really for it to work you need to heat your KCl/Li mixture in vacuum and above the BP of potassium (it's lower in partial vacuum than at atmospheric pressure, of course), thereby distilling off the potassium.

Someone here did this with Li/CsCl (search for it...)

TheChemINC - 25-2-2012 at 10:59

thats interesting..... i didnt know that it would work better in a vaccum. but i guess it would work better if it was void of O2 so it wouldnt oxidise. but when i did it, it wasnt to collect any samples of potassium metal. im going to use the method that this thread explains. it was more just for the fun of it, and to show my chem teachers....

White Yeti - 25-2-2012 at 11:11

Quote: Originally posted by TheChemINC  
im going to use the method that this thread explains. it was more just for the fun of it, and to show my chem teachers....


Love the enthusiasm, but if you look at this thread, you will see that some people took MONTHS to get this to work. Albeit, the Raging Nurd made a video on the subject, but it undermines all the time that went into getting this method to work.

In short, don't get your hopes up. If you do get it to work, be sure to post some pictures:)

Waffles SS - 25-2-2012 at 11:13

Thanks everyone,
I found out this is impossible to get lithium metal by this method

blogfast25 - 25-2-2012 at 12:53

Quote: Originally posted by White Yeti  
Love the enthusiasm, but if you look at this thread, you will see that some people took MONTHS to get this to work. Albeit, the Raging Nurd made a video on the subject, but it undermines all the time that went into getting this method to work.

In short, don't get your hopes up. If you do get it to work, be sure to post some pictures:)


Nonsense, Yeti: the 'trailblazers' took some time to get it right at first but for anyone capable of following simple instructions and in possession of the required chemicals this is a walk in the park.

Bear in mind a 'K synthesis' takes 3 - 4 hours of simmering the reagent mix at 200 C to get those balls of K, that's all...

This reaction was considered for a long time to be mysterious, sensitive, 'Goldielocks like' etc etc but those days are long gone, trust me.

[Edited on 25-2-2012 by blogfast25]

[Edited on 25-2-2012 by blogfast25]

MyNameIsUnnecessarilyLong - 29-2-2012 at 22:29

Anyone here have experience with doing a large scale of this reaction? Something at least 10:1? My aim is really to do about 40:1

Is there an issue with contact area or temp regulation, and overall reaction time?

I recall people saying it works better to not stir the rxn much, but would something like an overhead stirrer be needed for larger scales?

watson.fawkes - 1-3-2012 at 04:16

Quote: Originally posted by MyNameIsUnnecessarilyLong  
Anyone here have experience with doing a large scale of this reaction?
If you've never scaled up a reaction to pilot scale, I would heartily recommend this one not be your first one.

If you insist, however, start with the ΔG of the reaction, an estimated reaction rate, and the heat capacities of the materials.

blogfast25 - 2-3-2012 at 06:53

Quote: Originally posted by watson.fawkes  
Quote: Originally posted by MyNameIsUnnecessarilyLong  
Anyone here have experience with doing a large scale of this reaction?
If you've never scaled up a reaction to pilot scale, I would heartily recommend this one not be your first one.



Seconded totally: never scale up if you haven't bench tested it yet. Are you equiped to reflux 2 L of kerosene (or equivalent) for 2 to 4 hours at 200 C? Do you have fire fighting procedures in place should things go south? A large enough mantle heater and reflux cooler? :o

Pok - 2-3-2012 at 07:01

I did it several times in 10:1 scale. It works. By the way, the patent also says "1 liter".
When I want more, I make two 1-liter-batches simultaneously. Yields about 70 grams in total.
Recently, it didn't work anymore. Some problems which I can't explain up to now. But if you were successful in making the small scale reaction, 1-liter-batches will also work. Don't use too fine Mg powder! Otherwise the hydrogen will evolve too fast and it can become extremely dangerous (inflaming hydrogen/shellsol aerosol mixture), especially in larger scale! Also, only do a large scale reaction in a suitable laboratory with fire safety equipment (against burning paraffins and burning alkali metals!).

Temperature control, reaction time and stirring method were the same as in small scale.

[Edited on 2-3-2012 by Pok]

Neil - 2-3-2012 at 09:22

Quote: Originally posted by watson.fawkes  
Quote: Originally posted by MyNameIsUnnecessarilyLong  
Anyone here have experience with doing a large scale of this reaction?
If you've never scaled up a reaction to pilot scale, I would heartily recommend this one not be your first one.

If you insist, however, start with the ΔG of the reaction, an estimated reaction rate, and the heat capacities of the materials.



Pffft what's the worse that could happen


<iframe sandbox width="420" height="315" src="http://www.youtube.com/embed/C561PCq5E1g" frameborder="0" allowfullscreen></iframe>

Oh... well other then that I mean...

MyNameIsUnnecessarilyLong - 2-3-2012 at 17:56

Quote: Originally posted by blogfast25  


Seconded totally: never scale up if you haven't bench tested it yet. Are you equiped to reflux 2 L of kerosene (or equivalent) for 2 to 4 hours at 200 C? Do you have fire fighting procedures in place should things go south? A large enough mantle heater and reflux cooler? :o



Yes to all of those. But I am planning to reflux it in an expendable thick-bottomed erlenmeyer on hotplate instead of rbf in mantle. Last time I used a rbf and the KOH severely etched the glass, in some places the glass was left less than a 1/16" thick.

I will have the set up in a heavy gauge steel cabinet. Any fire should be contained. The box also has large gaping holes with steel shutters on them so any fuel explosions shouldn't blow it apart. If anything escapes, there is nothing within 40 feet around or above it that isn't metal or concrete.

MyNameIsUnnecessarilyLong - 2-3-2012 at 17:57

Quote: Originally posted by Pok  
I did it several times in 10:1 scale. It works. By the way, the patent also says "1 liter".
When I want more, I make two 1-liter-batches simultaneously. Yields about 70 grams in total.
Recently, it didn't work anymore. Some problems which I can't explain up to now. But if you were successful in making the small scale reaction, 1-liter-batches will also work. Don't use too fine Mg powder! Otherwise the hydrogen will evolve too fast and it can become extremely dangerous (inflaming hydrogen/shellsol aerosol mixture), especially in larger scale! Also, only do a large scale reaction in a suitable laboratory with fire safety equipment (against burning paraffins and burning alkali metals!).

Temperature control, reaction time and stirring method were the same as in small scale.

[Edited on 2-3-2012 by Pok]


Thanks Pok. I will do a run at 1L first

blogfast25 - 3-3-2012 at 06:36

And do report back here, presto! We need all the help we can get...

Bhaskar - 4-3-2012 at 22:34

http://www.instructables.com/id/Make-Potassium-Metal/ here is the synthesis for the video.

Bhaskar - 11-3-2012 at 21:38

Here is the video for the synthesis-
http://www.instructables.com/id/Make-Potassium-Metal/

Shit, sorry for the extra post, and there isn't an edit option for it!

[Edited on 06-10-2011 by Bhaskar]

White Yeti - 12-3-2012 at 16:18

there is, the top right hand corner, hit edit, and !delete this message! to get rid of the second post.

hames - 13-3-2012 at 04:31

hi,I got hold of about 150mls of t-butanol but its azeotropic is there anyway of purifying and drying it without using sodium wire.can I freeze it to separate it out or can I use it in the potassium synthesis as is.

garage chemist - 13-3-2012 at 06:48

I would dry it with potassium carbonate: add plenty of it and magnetically stir for a few hours, decant the liquid, separate the heavy aqueous K2CO3 solution in a separatory funnel if necessary, add some fresh K2CO3 and stir again, if the K2CO3 doesn't clump then you're done. If not, dry agin with fresh K2CO3.
A little residual water in the tert-butanol shouldn't hurt since the KOH contains 15% water anyway. K2CO3 doesn't remove all of the water, keep that in mind.
Anhydrous t-BuOH can be prepared from the predried product by dissolving sodium into it (doesn't have to be wire) and distilling.

[Edited on 13-3-2012 by garage chemist]

blogfast25 - 13-3-2012 at 07:32

Quote: Originally posted by hames  
hi,I got hold of about 150mls of t-butanol but its azeotropic is there anyway of purifying and drying it without using sodium wire.can I freeze it to separate it out or can I use it in the potassium synthesis as is.


What's the azeotropic water content? If it's not too high I'd use the product as such. The first part of the reaction is about reacting away most of the water anyway and the amount of additional water from your t-butanol shouldn't bother too much. At worst yield of K might be a little lower...

garage chemist:

Any progress on synthing longer chain 2-methyl t-alcohols?



[Edited on 13-3-2012 by blogfast25]

AndersHoveland - 13-3-2012 at 10:00

Quote: Originally posted by Waffles SS  
does this method is usable for making lithium metal?


Although this method has worked to make elemental potassium, it may likely not work for making lithium.

Lithium ions are more acidic, so would tend to form somewhat more covalent bonds with hydroxide ions. Lithium ions are also much smaller than the bulkier potassium ions, so the crystal lattice energy with hydroxide ions may be much greater. In other words, the formation of LiOH is significantly more favorable than KOH.

That is what is so interesting about this reaction. Potassium is usually a much more reactive element than lithium, and more difficult to make. But this reaction takes advantage of the unique reactivity differences of potassium.

But you could always use the potassium you have made to reduce lithium chloride to metallic lithium.

LiCl + K --> KCl + Li

blogfast25 - 13-3-2012 at 10:31

Quote: Originally posted by AndersHoveland  
Quote: Originally posted by Waffles SS  
does this method is usable for making lithium metal?


Although this method has worked to make elemental potassium, it may likely not work for making lithium.

Lithium ions are more acidic, so would tend to form somewhat more covalent bonds with hydroxide ions. Lithium ions are also much smaller than the bulkier potassium ions, so the crystal lattice energy with hydroxide ions may be much greater. In other words, the formation of LiOH is significantly more favorable than KOH.



Firstly, AFAIK no one has attempted reduction of LiOH by Mg, catalysed by t-alcohols, so we don't really know. LiOH is of course quite a bit harder to get than NaOH or KOH, at least for the hobbyist.

I doubt if lattice energy will play a huge part here: the STP HoF for LiOH is - 485 kJ/mol, for KOH it's - 425 kJ/mol (both values NIST webbook). That means that for LiOH the reduction with Mg to Li plus MgO plus H2 is still thermodynamicaly favourable (but slightly less so).

Should the reduction of LiOH prove to be impossible with the t-alcohol catalysed mechanism, the more likely reason would be reduced solubility of Li t-butoxide in non-polar solvents, vis-a-vis the solubility of K t-butoxide in equal conditions. That's an assumption, of course...

garage chemist - 13-3-2012 at 11:13

I have synthesized 2-methyl-2-hexanol about a year ago, but then neglected the potassium production and the little bottle of grignard-derived tertiary alcohol has been gathering dust until now.
Just one hour ago I started a batch using 3g grignard-grade Mg turnings (in contrast to my successful batch that used fine Mg powder), 6g KOH and 1ml tert-heptanol in 50ml Shellsol D70.
There was hydrogen and smoke production at the beginning but there's no potassium in sight one hour later. It doesn't seem to be a miracle catalyst.
Also, each drop of liquid that falls back into the flask from the dimroth condenser coil makes a little steam explosion. The alcohol clearly tends to volatilize from the reaction mixture despite the 141°C boiling point.
If this batch works I could try sticking two carbons more on the catalyst molecule, but I would need 1-hexanol to prepare the alkyl bromide for the grignard, and I don't have that.

blogfast25 - 13-3-2012 at 12:28

GC:

It would be really strange if 2-methyl-2-hexanol was shown not to work!

I acquired dihydromyrcenol recently, which also is a 2-methyl t-alcohol, a C8 if I recall well, but haven't found time to test it yet...

garage chemist - 13-3-2012 at 13:39

Reaction mixture was left to cool after 3 hours of vigorous reflux and the solids inspected with spatula, forceps and by throwing portions of it into water. Absolutely no potassium has formed, not even tiny particles. The magnesium was still present as mostly unchanged 1 mm sized grains surrounded by initially melted and then solidified crumbly KOH.
Thus I found that even this catalyst doesn't allow potassium production with magnesium filings, at least when using the typical catalyst concentration. This sucks since Mg powder is watched here and too risky to buy.

I could try a batch with increased catalyst concentration later.

AndersHoveland - 13-3-2012 at 16:03

Apparently under some reaction conditions, sterically hindered alcohols (such as tert-butanol) are much less vulnerable to reduction than non-sterically hindered alcohols (such as isopropanol).
Quote:

The sterically hindered tertiary butyl group imparts stability compared to primary and secondary alcohols. As a result, the solubility and oxidative stability characteristics provide many industrial applications as a reaction and process solvent and chemical intermediate. It is used as a non-reactive solvent for chemical reactions.

blogfast25 - 13-3-2012 at 17:22

garage chemist:

Wow, that's pretty disheartening news: if a C6 t-alcohol doesn't work, higher chain lengths aren't likely to fair much better. I wonder what the problem here is: might the longer alkyl tail actually be getting 'in the way', making the OH group less accessible?

I wonder if you'd be willing to let me have a couple mL of your product, for corroboration on my part? Remember that Len1 years ago very decisively stated that the t-butanol method didn't work and how he was proven completely wrong by POK and so many of us... For good science really someone should confirm your results.

[Edited on 14-3-2012 by blogfast25]

garage chemist - 13-3-2012 at 23:54

I have a few ideas that I should try: preactivating the Mg by refluxing it in Shellsol with some tert-alcohol like NurdRage has shown is one of them, as well as adding the catalyst in small portions over time during reflux.
I saw that NurdRage has had success with relatively coarse Mg turnings, which I find very remarkable since switching from powder to turnings did not work for me at all.

Yes, I can send you some of the alcohol once I've made a few more experiments. Only about 20g are present here ATM but if I or you can get this to work I will synthesize more of it.

hames - 14-3-2012 at 00:10

blogfast the percentage is around 87% I believe but the drum I got it out of says 99% tertiary butanol but I looked on the companies website (united initiators)and it says their product is azeotropic tert butanol maybe they mean the 87% which is tba is 99% pure also it doesn't crystalize at 25 degrees.

garage chemist,could I use anhydrous magnesium sulfate as I have it on hand,I only have 150mls as its near impossible to buy I don't want to ruin it so I might try it as is.

I've also decided that I'm going to try make a bit as well,I have heaps of n-butanol,can I make t-butanol from bromobutane in a grignard? and would I then react the butyl magnesium bromide with acetone.

blogfast25 - 14-3-2012 at 05:56

Quote: Originally posted by garage chemist  
I have a few ideas that I should try: preactivating the Mg by refluxing it in Shellsol with some tert-alcohol like NurdRage has shown is one of them, as well as adding the catalyst in small portions over time during reflux.
I saw that NurdRage has had success with relatively coarse Mg turnings, which I find very remarkable since switching from powder to turnings did not work for me at all.

Yes, I can send you some of the alcohol once I've made a few more experiments. Only about 20g are present here ATM but if I or you can get this to work I will synthesize more of it.


If I understand well (maybe not) you're now using a grade of Mg that hasn't given satisfaction in the past? I've only ever used one grade and it's a fairly course powder, reagent grade. Never had to resort to 'activating'. If you're going to 'activate' the Mg, why not use IPA in a bit of Shellsol, then discard the IPA/Shellsol, wash the Mg with clean Shellsol, then add the reagents/solvent?

Regards how to add the catalyst, as you probably know I'm convinced it can be added right from the start without need for the 'ritualised addition sequence' which strikes me as chemical superstition. Several experiments show that 'one pot' works just as well w/o any discernible difference between patent/POK and 'one pot'.

I'd love to test your alcohol at some point.
Quote: Originally posted by hames  
blogfast the percentage is around 87% I believe but the drum I got it out of says 99% tertiary butanol but I looked on the companies website (united initiators)and it says their product is azeotropic tert butanol maybe they mean the 87% which is tba is 99% pure also it doesn't crystalize at 25 degrees.

garage chemist,could I use anhydrous magnesium sulfate as I have it on hand,I only have 150mls as its near impossible to buy I don't want to ruin it so I might try it as is.

I've also decided that I'm going to try make a bit as well,I have heaps of n-butanol,can I make t-butanol from bromobutane in a grignard? and would I then react the butyl magnesium bromide with acetone.


hames: as a starting point I would try the alcohol as such. Should it not lead to the desired result, try drying. Just my two cents...

Bromobutane grignarded with acetone would give you 2-methylhexan-2-ol, not t-butanol, which is what garage chemist did.

Using bromoethane grignarded with acetone gives 2-methylbutan-2-ol (aka 2M2B), the only other (besides t-butanol) tertiary alcohol that we know for certain also works: I use it instead of t-butanol.



[Edited on 14-3-2012 by blogfast25]

garage chemist - 14-3-2012 at 07:43

I'm not using the turnings that didn't work before (those were selfmade), I'm now using "grignard grade" 99,8% Mg turnings, and I haven't tried these before.

garage chemist - 14-3-2012 at 09:56

New batch is running. This time, 40ml Shellsol D70 was used, and 3g grignard Mg turnings were refluxed in it with addition of 0,3ml tert-heptanol for 30 minutes. After this, the solvent was slightly turbid.
It was left to cool slightly, and 6g KOH were added.
After resuming heating, there was vigorous bubbling and smoke evolution, and then all of a sudden the mixture frothed up and emitted blue smoke out of the condenser. There was also blue froth being thrown up until the top of the condenser, the mixture assumed a blue color for just a few seconds and then returned to turbid yellowish. I was very surprised, this was the first time I saw something emitting blue smoke unexpectedly!

I added another 0,3ml tert-heptanol and continued refluxing.
Let's see what this witches' brew will do next. Has anyone ever seen this reaction produce a blue smoke and froth?
The new catalyst seems to be doing at least something ...

blogfast25 - 14-3-2012 at 10:42

Understood on the new Mg.

But blue smoke?!? Holy Moly...

Let's see if any K results. Your t-heptanol was purified properly, right? I'm thinking residual bromobutane might wreak havoc with any formed K but that's just speculation right now.

Could the blue be finely dispersed fresh K?

[Edited on 14-3-2012 by blogfast25]

garage chemist - 14-3-2012 at 11:02

The tert-heptanol was isolated and purified to the best of my skill and knowledge, and I am quite sure it does not contain any residual bromobutane. The product was constant boiling, and the forerun was the azeotrope with water which was dried and redistilled.
The blue froth did not react violently with water, it didn't even bubble.

The batch looks very different now than the last time, it went kinda "dark", like my successful batch. I broke up the hard solid cake with a spatula, added another 0,3ml tert-heptanol and continued refluxing. It looks as if there are tiny potassium droplets forming.
Breaking up the solids and stirring during the reaction seemed to really speed things up, seems like this is important with coarse Mg.

blogfast25 - 14-3-2012 at 12:51

Quote: Originally posted by garage chemist  

The batch looks very different now than the last time, it went kinda "dark", like my successful batch. I broke up the hard solid cake with a spatula, added another 0,3ml tert-heptanol and continued refluxing. It looks as if there are tiny potassium droplets forming.
Breaking up the solids and stirring during the reaction seemed to really speed things up, seems like this is important with coarse Mg.


In my experience, coalescence of any formed K into globules is what takes by far the longest time with this method. Not sure whether this is affected by Mg granulometry.

garage chemist - 14-3-2012 at 12:52

Results: only an extremely small amount of potassium has formed, just two or three 1mm-sized spheres. Most of the magnesium and KOH was still unreacted.
The flask was also heavily attacked by the molten KOH and now has a crack on the bottom, so it has to be thrown away.
Potassium has started forming early but the reaction then stopped dead in its tracks. Very strange.

blogfast25 - 15-3-2012 at 05:42

It certainly is very strange. Annoying also, this kind of 'halfway house' result... In any case it doesn't seem to constitute an improvement over t-butanol or 2M2B.

That 'glitch' at the start keeps bothering me though...

[Edited on 15-3-2012 by blogfast25]

[Edited on 15-3-2012 by blogfast25]

Lambda-Eyde - 15-3-2012 at 13:52

Quote: Originally posted by garage chemist  
Results: only an extremely small amount of potassium has formed, just two or three 1mm-sized spheres. Most of the magnesium and KOH was still unreacted.
The flask was also heavily attacked by the molten KOH and now has a crack on the bottom, so it has to be thrown away.
Potassium has started forming early but the reaction then stopped dead in its tracks. Very strange.

That's disappointing, gc. Both on the results and on the fate of your flask. I'm worried about damaging my ground glass erlenmeyers when I decide to have a go at this reaction. At the moment I only have grignard magnesium (but no ether :P), but I'm also getting some powder soon. I'll be trying out both, together with paraffin and some really old KOH.

blogfast25 - 16-3-2012 at 05:50

Quote: Originally posted by Lambda-Eyde  

I'm worried about damaging my ground glass erlenmeyers when I decide to have a go at this reaction. At the moment I only have grignard magnesium (but no ether :P), but I'm also getting some powder soon. I'll be trying out both, together with paraffin and some really old KOH.


Don't: almost no one has really complained about damage to glass ware (hint: we're not in aqueous media here).

Grignard magnesium should do nicely.

hames - 17-3-2012 at 17:20

blogfast is it possible to use methylated spirits when making bromothane its very expensive to get pure ethanol here,only the stuff you drink but it over $60 for probly 700mls would there be other bromides formed when using metho.

[Edited on 18-3-2012 by hames]

blogfast25 - 18-3-2012 at 06:49

Quote: Originally posted by hames  
blogfast is it possible to use methylated spirits when making bromothane its very expensive to get pure ethanol here,only the stuff you drink but it over $60 for probly 700mls would there be other bromides formed when using metho.

[Edited on 18-3-2012 by hames]


If the denaturing agent used is methanol then that would blow off as bromomethane, I'd imagine. TBH, I'm no expert on synthing bromoethane, my most recent experience being a class room experiment 30 yrs ago! But methylated spirits (the colourless variety) would be my precursor of 'choice' if I had to synth it today. Nothing a little distillation couldn't do for good purity.

Careful with these haloalkanes, few of them are particularly kosher when it comes to health.

nora_summers - 18-3-2012 at 08:38

I'm having some trouble making K.

I started with 20mL of baby oil, 2 grams of magnesium and 5 grams of KOH with 0.7mL of 2-methyl-2-propanol. I heated it up to 220 celsius with a condensor and a bubbler.

nothing happened after i left it for 7-8 hours. sometimes it turned yellow but 4 out of 6 times it remained clear. No potassium though.

What am i doing wrong?

blogfast25 - 18-3-2012 at 10:29

Did you at least get hydrogen generation early on? If not, chances are your magnesium isn't active enough.

nora_summers - 18-3-2012 at 12:51

i got bubbling early on, so i think the magnesium is ok.

garage chemist - 18-3-2012 at 13:18

I always had the same result with Mg filings, both selfmade and bought: vigorous hydrogen evolution at the beginning, but no potassium later. It's a sure sign that the magnesium is too coarse. Try it with Mg powder.

nora_summers - 18-3-2012 at 16:11

how fine does it have to be? i don't want to order it and find out that is too coarse as well.

Redroy - 18-3-2012 at 23:35

I've had the same problems trying this myself. Bubbles away steadily as the temp increases and after 4-5 hours nothing. I've tried several different types of Mg, from granules, to shavings and powder but they've all been very old samples. Getting Mg powder here in NZ seems next to impossible so I've got a hold of a block of 99.9% Mg I'm gonna try make some powder "freshly". Hopefully that's my only problem.

On the note of glassware I've noticed on the bottom of mine (from this experiment) is some sort of clear hard crud, which I can't seem to move. Nothing I try will get rid of it. Anyone else have this issue?

blogfast25 - 19-3-2012 at 06:11

Quote: Originally posted by nora_summers  
how fine does it have to be? i don't want to order it and find out that is too coarse as well.


Hard to say but mine, although unspecified in terms of granulometry, isn't really that fine, with the largest particles probably up to about 0.25 mm. I don't think a super fine grade is needed.
Quote: Originally posted by Redroy  

On the note of glassware I've noticed on the bottom of mine (from this experiment) is some sort of clear hard crud, which I can't seem to move. Nothing I try will get rid of it. Anyone else have this issue?


It's probably stating the blindingly obvious but have you tried conc. HCl?

[Edited on 19-3-2012 by blogfast25]

garage chemist - 19-3-2012 at 14:18

The Mg powder that worked for me had a particle size of 75 micrometers. I need to try this powder with my tert-heptanol, to see whether the alcohol is actually active and how fast the reaction goes.

Vinylogous - 21-3-2012 at 15:57

That's an interesting and slightly disappointing result with the tert-heptanol.

Is it possible that the magnesium alkoxide formed, (t-HepO)2Mg, is very insoluble, and essentially passivates the magnesium? Which stirring and agitating with a spatula would alleviate. It seems counterintuitive; that long alkane tail should theoretically make it easier to dissolve in paraffin. But it's worth some thought, as solubility is a rather complex matter, and often makes for paradoxical patterns.

I'm not sure how interested anyone is still in the rather-long-chain tert alcohols, but Fractionated Palm Oil is composed of a large percentage (can't find a suitable chart at the moment) of C8, C10, and C12 fatty acid triglycerides. It could be transesterified to fatty acid methyl esters, and possibly fractionally crystallized to obtain what is mostly methyl octanoate.

Reacting MeMgBr with methyl octanoate would afford 2-methylnonan-2-ol. (I know there is the thread specifically on alcohols, but it's buried a few pages back, and didn't want to necro it)

Additionally, butyl cellosolve (2-butoxyethanol) is readily available OTC online and cheap. No idea how the ether functionality would hold up to metallic K at various temperatures, but I know brake fluid was entertained as a coalescing fluid; 2-butoxyethanol by itself, or a derivative thereof, may be useful for this purpose. If one were really crackers, they could possibly even fashion a tert alcohol out of it (conversion to the 1-halo-2-butoxyethane, then Grignard with acetone), but I reckon that's way out of the scope of most of us here. Just jogging the brain juices. :P

[Edited on 22-3-2012 by Vinylogous]

blogfast25 - 24-3-2012 at 06:57

Quote: Originally posted by Vinylogous  


I'm not sure how interested anyone is still in the rather-long-chain tert alcohols, but Fractionated Palm Oil is composed of a large percentage (can't find a suitable chart at the moment) of C8, C10, and C12 fatty acid triglycerides. It could be transesterified to fatty acid methyl esters, and possibly fractionally crystallized to obtain what is mostly methyl octanoate.

Reacting MeMgBr with methyl octanoate would afford 2-methylnonan-2-ol. (I know there is the thread specifically on alcohols, but it's buried a few pages back, and didn't want to necro it)

Additionally, butyl cellosolve (2-butoxyethanol) is readily available OTC online and cheap. No idea how the ether functionality would hold up to metallic K at various temperatures, but I know brake fluid was entertained as a coalescing fluid; 2-butoxyethanol by itself, or a derivative thereof, may be useful for this purpose. If one were really crackers, they could possibly even fashion a tert alcohol out of it (conversion to the 1-halo-2-butoxyethane, then Grignard with acetone), but I reckon that's way out of the scope of most of us here. Just jogging the brain juices. :P

[Edited on 22-3-2012 by Vinylogous]


The possibility of using fractionated palm (coconut) oil for the purpose of obtaining C8 and higher 2-methylalkan-2-ol type t-alcohols has been discussed in the thread you mentioned.

As regards solvents with oxygen atoms, I've tried several and they all react with the potassium. I can't see something derived from butoxyethanol being much different.

Regards your point on metal alkoxides and their solubility: it's difficult to find data on that, which means we're driving blind here. The failure of t-heptanol has put a bit of a dampener on things...

[Edited on 24-3-2012 by blogfast25]

[Edited on 24-3-2012 by blogfast25]

hames - 24-3-2012 at 15:40

sorry for so much spoonfedding but I am a noob,would 4a molecular sieves be suitable for t-butanol also I have access to surfactants that are 100% c-8 to c-12 ethoxylated alcohols is their any way to extract the alcohol out of it,I get heaps of it and its thrown out as waste its a product called teric made by huntsman there are a few different ones but i have heaps of most types

[Edited on 24-3-2012 by hames]

AndersHoveland - 24-3-2012 at 21:55

Quote: Originally posted by blogfast25  

As regards solvents with oxygen atoms, I've tried several and they all react with the potassium. I can't see something derived from butoxyethanol being much different.


Ethers do not react with potassium, at least not at room temperature.

But in this reaction, I thought we wanted the tert-butyl ether to react. At least to form butoxide, which solubilizes the potassium ions.

The main reason tert-butyl alcohol is used seems to be that it is not so easily reduced like other alcohols.

blogfast25 - 25-3-2012 at 09:44

Quote: Originally posted by AndersHoveland  

Ethers do not react with potassium, at least not at room temperature.

But in this reaction, I thought we wanted the tert-butyl ether to react. At least to form butoxide, which solubilizes the potassium ions.

The main reason tert-butyl alcohol is used seems to be that it is not so easily reduced like other alcohols.


Room temperature is of no use. To obtain coalescence you need to be above the MP of K.

The main reason, at least going by the proposed reaction mechanism, that t-butanol (and 2M2B) work is that they form alkane soluble alkoxides with K and Mg.

nora_summers - 25-3-2012 at 18:29

I think my magnesium is pretty fine, so before I buy even finer magnesium, is there anything else I can try instead to make this reaction work? I tried shaking and stirring but that didn't do anything i could see.

CrEaTiVePyroScience - 14-4-2012 at 11:23

@UnintentionalChaos I have tried to make sodium with it and my friend also tried it but it didn't worked. Believe me don't try it , it will waste alot of your time. It just doesnt work for sodium =/

[b/]NOTE: But before you even do this experiment let me warn you: This ruins your glass equipment I was surprised after making seven times potassium metal that my glass was extremely thin , unusable. I figured out this is because potassium hydroxide is corrosive to glass. So don't use your new glassware like I did , use old glassware.[b/]

For me secondary alcohols as isproponal so I used tertiary alcohols as tertiary butanol as catalyst.
I haven't readed all 39pages of the forum so I might have mentioned things that other people already did , sorry if so.
But if you have any other questions about the proces I would love to tell you, just ask!

CrEaTiVePyroScience - 14-4-2012 at 11:27

@redroy Yes potassium hydroxide is corrosive to your glassware!!Text

White Yeti - 15-4-2012 at 10:06

I'm not sure if anyone already asked this, so forgive me if it has already been mentioned.
@blogfast25, you've had success with 2-methyl-2-butanol as catalyst. But this alcohol boils below 200C (which is from what I understand the temperature for this reaction to work).

Is it possible that the catalyst is simply being lost due to heating and that it's not being re-condensed completely? I understand that the condenser is meant to catch all the vapours, but nothing is perfect, and the amount of catalyst used is so small that this might be a legitimate source of error and a reason why many have tried this method, and failed.

blogfast25 - 15-4-2012 at 12:23

Quote: Originally posted by White Yeti  


Is it possible that the catalyst is simply being lost due to heating and that it's not being re-condensed completely? I understand that the condenser is meant to catch all the vapours, but nothing is perfect, and the amount of catalyst used is so small that this might be a legitimate source of error and a reason why many have tried this method, and failed.


Total reflux is total reflux: decent cooling catches anything that is basically non-gaseous at RT. BTW, so far I've only used a modified graduated pipette (about 300 mm long, ID about 7 mm), wrapped in moist kitchen towel (keeping the kitchen towel moist by drizzling iced water on it from time to time!) as a "refluxer" [cough!]. Worked perfectly...

Woelen used a Liebig condenser with some air (instead of water) as cooling agent blown through it and got good quality metal w/o any surprises.

No, loss of catalyst through the cooler is one of the least likely reasons for failure IMHO.

Anyone with a minimum of determination, decent chemicals and some patience can do this succesfully...



[Edited on 15-4-2012 by blogfast25]

Pok - 16-4-2012 at 12:01

Quote: Originally posted by White Yeti  
Is it possible that the catalyst is simply being lost due to heating and that it's not being re-condensed completely?


I think that this problem can only occur at the beginning (t-butanol addition). Very soon the reflux becomes weaker and after some time you even don't smell the alcohol anymore. Maybe at this point the alcohol is already bound as a compound (catalyst mechanism) in the liquid mixture - and doesn't exist in a free state. Some time after the t-butanol addition the reflux doesn't seem to be crucial. I always let the toilet paper dry on the outside of my glass pipe after a while....and no t-butanol loss seems to result.

Redroy - 16-4-2012 at 15:48
Quote:

@redroy Yes potassium hydroxide is corrosive to your glassware!!


Yes I know it's corrosive, however it looks like a deposit, not corrosion / pitting.

blogfast25 - 17-4-2012 at 11:55

Quote: Originally posted by Redroy  


Yes I know it's corrosive, however it looks like a deposit, not corrosion / pitting.


Post reaction the bottom of your reactor is covered with mainly MgO. It dissolves readily in dilute HCl. I've never experienced damage to the (borosilicate) glass. Remember that we're in strict anhydrous conditions here and well below the MP of pure KOH.

ALWAYS make sure during clean-up that you've reacted away any residual potassium, best by using alcohol or IPA. Then clean your reactor with dilute HCl.

alkalimetals - 26-4-2012 at 08:15

If I use as solvent C11-C13 alkanes with 0.001% of aromatics does it work?

blogfast25 - 27-4-2012 at 11:53

Decane has been used by nurdrage with good results. Aromatics do not seem to be a problem either (Shellsol D contains some and is the 'solvent' of the original patent).

alkalimetals - 28-4-2012 at 23:33

Thank you very much! I'll try to synthetize potassium metal and I'll post it here :)

nora_summers - 12-5-2012 at 10:38

I finally made some potassium! It was lots of little spheres (less than 1mm) but it was clearly potassium and popped and flamed when i put them in water!

I just had to add the alcohol drop by drop and it finally started making potassium. to total amount i added was 0.5mL.

I also boiled my baby oil at 220 celsius with nothing in it (no KOH or Mg or alcohol) for a few hours and then letting it cool. I'm not sure if this did anything but i thought i should mention it here.

I also want to report my glassware seems etched now :( in reading the thread i think the glassware gets etched if you use mineral oil or baby oil for the solvent, but if you use shellsol d70 it does not get etched. can anyone confirm this? as i do not have shellsol d70 to compare to.

blogfast25 - 12-5-2012 at 11:10

Nora:

If you keep refluxing the mini globules eventually coalesce into larger ones. It's this coalescencing process that takes up most of the time.

Boiling baby oil will dry it. But it's probably pretty dry to start with.

I've used Sellsol D and kerosene and didn't get any etching with either of them. Not sure about baby oil...

nora_summers - 12-5-2012 at 12:50

maybe thats why people are getting inconsistent results. some people are using baby oil, mineral oil or stuff like that. and others are using shellsol and kerosene. might explain why some are etching and that some people have to add the alcohol drop by drop instead of all at once.

jamit - 13-5-2012 at 00:39

@blogfast25

Does it matter why type of kerosene you use? Can I use the kerosene for heating? Is there anything particularly different about using Kerosene as the solvent as opposed to other solvent you have tried?:)

blogfast25 - 13-5-2012 at 06:03

Quote: Originally posted by jamit  
@blogfast25

Does it matter why type of kerosene you use? Can I use the kerosene for heating? Is there anything particularly different about using Kerosene as the solvent as opposed to other solvent you have tried?:)


Not as far as I know (I used 'deodorised' lamp oil).

Yes.

No. As long as the 'solvent' is inert and has a boiling point (or range) near or above 200 C.

watson.fawkes - 13-5-2012 at 09:59

Quote: Originally posted by jamit  
Is there anything particularly different about using Kerosene as the solvent as opposed to other solvent you have tried?:)
The recommended solvents have been treated by hydrogenation, so there are quite low percentages of alkenes and aromatics. Ordinary kerosene still has significant quantities of these. For the reaction itself, I imagine this only affect yields.

It may, however, have something to do with the glass etching reported, as the combination of a double bond which can be oxidized, atomic potassium, and the mixed oxides within glass doesn't seem like a completely inert combination to me.

blogfast25 - 13-5-2012 at 10:58

Nurdrage used tetralin once, without any problems. The double bonds left in there aren't really aromatic but still. Double bonds don't seem to have much effect, 'within reason' at least...

watson.fawkes - 13-5-2012 at 14:44

Quote: Originally posted by blogfast25  
Nurdrage used tetralin once, without any problems. The double bonds left in there aren't really aromatic but still. Double bonds don't seem to have much effect, 'within reason' at least...
I am admittedly reaching for a hypothesis. One solvent has reports of etching, another doesn't. I could believe that long chain olefins behave differently than cyclic compounds. It certainly might not be this, but it's the only thing so far reported that seems to have any correlation.

blogfast25 - 14-5-2012 at 05:13

How about 'quality of glass ware'? A priori I would not expect much difference between one type of glass and another in terms of alkali resistance but who knows?

Polesch - 15-5-2012 at 09:48

How can you explain the thermodynamics involved in this reaction? If the reaction is as stated in NurdRage's video: 2Mg + 2KOH -> 2K + H2 + 2MgO

The half-reaction has to be 2K+ + Mg -> 2K + Mg2+? Which is impossible? Considering the electrode potentials.

http://www.chemguide.co.uk/physical/redoxeqia/predict.html

If this reaction is to work, there are to be a more feasible mechanism. Am I wrong here?

barley81 - 15-5-2012 at 11:14

A half-reaction gives no indication of the whole reaction's spontaneity. For example, should the reaction of zinc and magnesium (Zn<sup>2+</sup> + Mg -> Zn + Mg<sup>2+</sup>;) be nonspontaneous because Zn<sup>2+</sup> + 2e<sup>-</sup> -> Zn has a negative potential? You must look at the cell voltage, not the half-reaction potentials. If the cell voltage is positive, then delta G is negative and the reaction is spontaneous (but does not necessarily occur at an appreciable rate).

It is probably due to the formation of MgO being so favorable that the reaction can proceed with an appropriate catalyst.

[Edited on 15-5-2012 by barley81]

blogfast25 - 15-5-2012 at 12:26

The reaction:

KOH(s) + Mg(s) == > K(l) + MgO(s) + ½ H2(g)

is thermodynamically favourable (the Standard Heat of Reaction has been calculated elsewhere in the thread). At 200 C it would normally not proceed though. That’s where the catalyst comes in: it reduces the activation energy of the reaction so that it can proceed at much lower temperatures (such as 200 C).

Half-cell potentials are a very poor guideline here: we’re not working in solution. You really need to calculate the actual ΔG in the relevant conditions, not in conditions that don’t apply.

A detailed proposes reaction mechanism, including the role of the catalyst, has been described higher up in the thread too…

Wizzard - 7-6-2012 at 13:53

My first attempt!!

I distilled my own t-butyl alcohol from Turbo 108 octane booster, after letting the solution sit, taking the lighter fluids (leaving behind the dark, staining messy liquid), mixing with water, freezing the solution (which separated like oil and water), then distilling what WAS ice to get the required alcohol...

I mixed to NurdRage's specifications- 2.5g magnesium (Kind of old, but was refluxed and made shiny after distilling with hot mineral oil and some t-butyl alcohol) and 5g of very dry KOH into about 30mL of hot, distilled mineral oil (I previously distilled to removed lighter oils- boiled at around 230*C)

Initially, it boiled vigorously and was opaque. I figured this was the stage where it released H. I then added dropwise some t-butyl alcohol, which also greatly increased boiling, which then came to a murmur, even under increased temperature. The heated vessel would bump every minute or so, with a spray of mist, condensing and dripping into the hot oil.

8 hours later, I was left with an opaque oily solution, with some hard magnesium at the bottom. I noticed, adhered to my stir rod, was some nice shiny Mg. But no K. After letting cool overnight, and then checking it out- I dumped the contents into an open vessel, and tool some out and dropped it into water- No fizzing, popping, bubbling, nothing.

The solution came out in 2 layers- The light amber oil, opaque with KOH I would guess, was less viscous than the lower layer, which was thicker and whiter.

Any help would be appreciated... Maybe my alcohol was impure, my mineral oil had problems? I'll try cleaner Mg, and kerosene next time. But kerosene and parrafin will need perfect supervision, as opposed to "I'm in the next room, checking any 5 minutes" type.

blogfast25 - 9-6-2012 at 07:08

You're using fairly 'dodgy' ingredients, thereby possibly introducing a panoply of possible errors. Any idea of temperature during the run.

'Turbo 108 octane booster' contains t-butyl alcohol? Interesting!

elementcollector1 - 11-6-2012 at 21:20

Urgh... I have access to pretty much everything but the KOH. Why is the state of Washington so lacking in scientific supplies?

Anyway, the route I think I'll go is thus:

-Vaseline as main liquid, because of density (compared to molten K), 20mL.
-T-butanol distilled from the Turbo Octane Booster 108, 1mL.
-KOH from... wherever I'll get KOH. Electrolysis?
-Magnesium from shaved magnesium firestarter block.

Questions:

I will have a Graham coiled condenser shortly, so how do I set this up to condense the fumes from the reaction (while still letting H2 escape)? Pretty sure it involves hooking the condenser to the top of the flask, placing Al foil loosely on top, and running water (or air?) through. Or a wet paper towel, I saw that a few pages back.

How fine, in your opinion, should the magnesium be for best results? I have a ball mill and/or hacksaw if entirely necessary.

Is there a good way to 'clean' any K formed without using toluene?

Are there any easier substitutes for the reagents I'm using? I have what is stated to be 99.9% mineral oil, but K doesn't float in this.

Wizzard - 12-6-2012 at 05:10

Sure does, according to multiple Google sources :)

http://www.hotrodders.com/forum/octane-booster-info-124750.h...
Quote:

Turbo Octane Boost 108
(No percentages given)
Methanol
t-Butyl alcohol


I distilled the t-butyl alcohol out with some heat, about 90*C, then froze it- It froze, the oil that came over with it did not. Also, letting the Turbo 108 sit for an extended period (after purchasing and transporting it) settled out all the garbage.

As for the K, I refluxed at around 210*C, just enough for the mixture to boil and occasionally bump.


[Edited on 6-12-2012 by Wizzard]

MyNameIsUnnecessarilyLong - 15-6-2012 at 04:12

Quote: Originally posted by Wizzard  
Sure does, according to multiple Google sources :)

http://www.hotrodders.com/forum/octane-booster-info-124750.h...
Quote:

Turbo Octane Boost 108
(No percentages given)
Methanol
t-Butyl alcohol


I distilled the t-butyl alcohol out with some heat, about 90*C, then froze it- It froze, the oil that came over with it did not. Also, letting the Turbo 108 sit for an extended period (after purchasing and transporting it) settled out all the garbage.



How much t-butanol did you manage to distill from it?

blogfast25 - 15-6-2012 at 04:58

Quote: Originally posted by MyNameIsUnnecessarilyLong  


How much t-butanol did you manage to distill from it?


Also, was any identifying test (density, MP or BP) carried out on the product?

Wizzard - 15-6-2012 at 05:56

Only about 2ML, I cut the operation short when I realized I had enough, it was coming over very slow. I tested it's approximate boiling point and melting point, it froze around 10*C (it was a fairly thick liquid, almost gel-like, in relation to the lighter alcohols which also came across but were removed, they did not freeze and I simply extracted the frozen substance from the rest after putting the bottle in the fridge). Boiling was right very brisk when moderate heat was added (I did this with a cold finger to re-distill the small amount, just to double purify it, neglecting efficiency and waste).

I have more distilling now, I had a 'batch error' where the plastic vessel I had the gasoline additive in apparently did not agree with the product- It promply leaked like a sieve, and my work area smelled of gas for some number of hot days. That was the reason for cancellation of the previous distillation process :)

blogfast25 - 15-6-2012 at 07:02

Sounds like the catalyst wasn't the source of your problems...

Wizzard - 15-6-2012 at 13:15

Anything you'd recommend? I'm going to re-run the process with the same ingredients, once I distill more t-butyl alcohol. See if the same problems arise... I have new ingredients on the way.

Seventh cavalry - 16-6-2012 at 22:54

Looks good, any one have translated or something ?

blogfast25 - 17-6-2012 at 07:54

Quote: Originally posted by Wizzard  
Anything you'd recommend? I'm going to re-run the process with the same ingredients, once I distill more t-butyl alcohol. See if the same problems arise... I have new ingredients on the way.


Try 'one pot'? Just start with all ingredients mixed in your reactor, then start heating. It's what I do.
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