| Pages:
1
..
3
4
5
6
7
..
13 |
ballzofsteel
Harmless
Posts: 31
Registered: 13-3-2004
Member Is Offline
Mood: No Mood
|
|
Nitrate patent
Hey Bromic,
Did you take a look at the patent I posted
further on up the thread regarding reduction of the nitrate with Sodium carbonate??
It is fairly comprehensive,explaining in detail,construction materials ect.
Some real good info for you there man.
Pretty please,give it a read.
Fuse them salts,lower the temps needed
collect you nitric acid.
|
|
|
BromicAcid
International Hazard
Posts: 3246
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
Correcting my mistakes
| Quote: |
Then after you get your fill you put it in, jeeze, I forget the exact name so you're going to have to settle for a phonic equivalent, linindale
or something of that nature, regardless it is an inert substance, I think a paraffin of some sort with a low density around .56 and apply heat. The
sodium will melt and float to the surface leaving hydroxide behind from there scoop it back up and store under your final storage solution.
|
I actually looked up the procedure in the library, it's actually for making lithium but the principle should be the same since we are working in
terms of physical properties. You would take your Na with NaOH contaminates and put it in a paraffin bath. The sodium melts and floats to the
surface and the NaOH stays on the bottom. The thing bout the ligroin is specifically related to the lithium procedure that this was written
for. The density of this fraction of petroleum ether is only .56 g/ml which seems to be very slightly higher then the .53 g/ml for lithium. I guess
at best it might make a suspension. It recommends storing Li in a container filled to the brim of this stuff regardless.
|
|
|
The_Davster
A pnictogen
Posts: 2861
Registered: 18-11-2003
Member Is Offline
Mood: .
|
|
I used an alcohol not a bunsen burner to melt the sodium hydroxide, took a long time though. Also it seems to me that crystall drano has a lower
melting point than pure sodium hydroxide. It must be mixed with some sort of oxidizer because if a popsicle stick is dipped into the molten draino it
catches fire once removed.
|
|
|
Saerynide
National Hazard
Posts: 954
Registered: 17-11-2003
Location: The Void
Member Is Offline
Mood: Ionic
|
|
Off Topic, but....
Neat!! I want to try the flaming popsicle stick thing now 
"Microsoft reserves the right at all times to monitor communications on the Service and disclose any information Microsoft deems necessary to...
satisfy any applicable law, regulation or legal process"
|
|
|
BromicAcid
International Hazard
Posts: 3246
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
The commercial draino is somewhat hydrated, that is the main impurity that I know of that causes it to melt at a lower temperature. As for
the flaming popsicle stick I think there was a thread posted here about it. How the hydration of NaOH can start a fire. Put a popsicle stick that
has water throughout it into molten NaOH and watch it make excessive energy from hydration and set it on fire
|
|
|
Polverone
Now celebrating 21 years of madness
Posts: 3186
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline
Mood: Waiting for spring
|
|
Drano contains some sodium nitrate (as mentioned upthread) as well as some sodium chloride, it appears:
http://householdproducts.nlm.nih.gov/cgi-bin/household/brand...
PGP Key and corresponding e-mail address
|
|
|
BromicAcid
International Hazard
Posts: 3246
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
Wow, I guess I was mistaken about water of hydration being the main impurity.
My bad. 
Regardless, I still stand by my belief that the inflamation of the wood in question is caused by the inheret moisture in the wood being acted upon by
the hot molten hydroxide.
|
|
|
Saerynide
National Hazard
Posts: 954
Registered: 17-11-2003
Location: The Void
Member Is Offline
Mood: Ionic
|
|
Maybe its like the "Gummybear goes to hell" thing with the molten KNO3 since Draino has NaNO3?
"Microsoft reserves the right at all times to monitor communications on the Service and disclose any information Microsoft deems necessary to...
satisfy any applicable law, regulation or legal process"
|
|
|
Strepta
Harmless
Posts: 44
Registered: 6-5-2004
Member Is Offline
Mood: No Mood
|
|
| Quote: | Originally posted by chemoleo
Bromic, your method doesn't seem all that different, except maybe the water addition.
I dont understand why you'd get metalic Na globules - everyone who's tried it (inc. myself), one gets a dark grey mass, with the occasional
yellow explosion from igniting H2/O2/Na.
It's not like your temperature is low (judging by the mark on the wooden bench  ), or that there is an oxygen deficiency in your local atmosphere (you wouldnt be writing this otherwise )
But seriously, I can't figure out why you'd get metalic sodium, as a nice little globule.
How about upscaling this?
Comments? |
|
|
|
patu
Harmless
Posts: 9
Registered: 9-4-2004
Member Is Offline
Mood: No Mood
|
|
I purify the sodium by heating it in just plain mineral oil I got at the supermarket. The sodium has a very high suface tension. The very pure sodium
rises to the top which creates a ball with a visible line between the shiny sodium and the dull sodium hydroxide. Even though the densities are
different the sodium really doesn't want to detach from the sodium hydroxide. I guess you could take a razor blade and just cut away the sodium.
|
|
|
Tacho
National Hazard
Posts: 582
Registered: 5-12-2003
Member Is Offline
Mood: No Mood
|
|
I must confess, embarrassed, that I also had a hot NaOH burn in my tongue. So, statistically, tongue burning is a major hazard in sodium making. Wear
googles and keep your mouth shut!
|
|
|
Saerynide
National Hazard
Posts: 954
Registered: 17-11-2003
Location: The Void
Member Is Offline
Mood: Ionic
|
|
You guys with all your alkali burns are scaring me. And I want to get lithium from batteries soon (summer hoilday is coming in 2-3ish weeks!!)
Edit: typo
[Edited on 13-5-2004 by Saerynide]
"Microsoft reserves the right at all times to monitor communications on the Service and disclose any information Microsoft deems necessary to...
satisfy any applicable law, regulation or legal process"
|
|
|
The_Davster
A pnictogen
Posts: 2861
Registered: 18-11-2003
Member Is Offline
Mood: .
|
|
Tacho: Ive tasted NaOH too. I was scraping sodium off the electrode with pliers
and the electrode sprung up and flicked some sodium hydroxide onto my tongue. I still cant think of why my tongue was out at that moment though...
|
|
|
Tacho
National Hazard
Posts: 582
Registered: 5-12-2003
Member Is Offline
Mood: No Mood
|
|
| Quote: | Originally posted by rogue chemist
Tacho: Ive tasted NaOH too. I was scraping sodium off the electrode with pliers
and the electrode sprung up and flicked some sodium hydroxide onto my tongue. I still cant think of why my tongue was out at that moment though...
|
See? See? Another one!
Hot NaOH is magnetically atracted to tongues!! Googles, gloves and MOUTHS SHUT!
|
|
|
Strepta
Harmless
Posts: 44
Registered: 6-5-2004
Member Is Offline
Mood: No Mood
|
|
High boiling organics with densities greater than 1
You need an inert liquid with a density of 1 g/cm3 or above with a boiling point of greater then 100C. This is the technique used to purify lithium
that I mentioned before, you melt the impure NaOH/Na mixture at the bottom and as it melts the pure-er Na will float to the top leaving the NaOH
behind. You could use something like nitrobenzene possibly. I think most chlorinated hydrocarbons will react with Na at these temps and that is the
massive drawback because most organic liquids that have a density of greater then 1 are halogenated hydrocarbons.
[Edited on 5/9/2004 by BromicAcid]
I thought I'd give a nitrated organic a try. I have toulene, so I prepared mono nitrotoluene (NT) according to Davis. It's a straightforward
nitration with mixed acid. I placed a small ball of Na in the NT in a test tube. It appeared to darken a bit. I heated it carefully-- the Na began to
react with the NT and soon all Na was consumed and the liquid, initially yellow, turned reddish brown. I suppose the Na is reducing the NT. Oh well, not much ventured..
[Edited on 16-5-2004 by Strepta]
[Edited on 16-5-2004 by Strepta]
|
|
|
Cyrus
Hazard to Others
Posts: 397
Registered: 24-4-2004
Location: Ancient Persia
Member Is Offline
Mood: No Mood
|
|
Magnetic NaOH
I have gotten NaOH on my tongue too, but not from electrolysis. I was doing a simple NaOH +Al reaction, and stuck my head too close to the bubbles.
Is SS ok for molten NaOH, and why do you all use nickel? I thought SS was dissolved very slowly by NaOH. Could you not use carbon, or even make a
carbon coating on your container with a candle?
Where can I get soda-lime glass to get
sodium that way?
|
|
|
BromicAcid
International Hazard
Posts: 3246
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
| Quote: |
Is SS ok for molten NaOH, and why do you all use nickel? I thought SS was dissolved very slowly by NaOH. Could you not use carbon, or even make a
carbon coating on your container with a candle?
|
I believe stainless reacts appreciably with NaOH(l) however I have no sources to back me up, some designs for castner cells call for cast iron which I
come across even easier, it holds up fairly well. I use nickel whenever possible because for as far as I can tell it is nearly invulnerable to molten
NaOH, I've used the same set of electrodes several times and no pitting and the molten NaOH does not turn colors from making nickel salts.
Carbon will die in NaOH(l) there is no getting around it, I used graphite rods as electrodes and it quickly formed as semi-metalic solution that
conducted electricity and thus accomplished no electrolysis.
As for where you can get soda lime glass, most everything made of glass that is not made for a lab is soda lime glass. But it needs to be thin, it
should have a partial vacuum within it, and it does break after a period of use. NASICON ceramics are the way to go for a membrane that permits only
Na though.
Edit: And Strepta, nice try, nice to see someone trying somthing an idea that I've put fourth, keep up the good work 
[Edited on 5/18/2004 by BromicAcid]
|
|
|
Cyrus
Hazard to Others
Posts: 397
Registered: 24-4-2004
Location: Ancient Persia
Member Is Offline
Mood: No Mood
|
|
I have tried electrolysis in Fe endcaps and Cu , and in food cans, and the food cans seem to withstand molten NaOH the best! In the other ones, it
changes to brown quickly, and if I stick any iron or copper wires into the melt, it will turn brown too...
BromicAcid, does that mean I could use the glass in a lightbulb? It is pretty thin and will withstand a vacuum. If only the wires inside of the
lightbulb touched the edge Then you could just plunk a lightbulb into the NaNO3
melt and connect it to your power source, as it already has a vacuum inside, run the cell, get the sodium, and crack the bulb open!
|
|
|
Saerynide
National Hazard
Posts: 954
Registered: 17-11-2003
Location: The Void
Member Is Offline
Mood: Ionic
|
|
Inside a light bulb isnt a vacuum. Theres a noble gas in there, I cant remember which one though.
But I was also thinking about using lightbulbs to melt or heat stuff in, since I dont have pyrex, and if light bulbs can withstand constant heating, I
hope they can withstand a gas stove
Edit: I was going to open a light bulb by removing the connector and taking out all the crap in it, to get a flask like container. But now come to
think of it, Im kinda worried that H2 might build up in the bulb (since it has a narrow opening) and with the Na forming, it might turn the lightbulb
into a glass pipebomb
[Edited on 20-5-2004 by Saerynide]
"Microsoft reserves the right at all times to monitor communications on the Service and disclose any information Microsoft deems necessary to...
satisfy any applicable law, regulation or legal process"
|
|
|
Esplosivo
Hazard to Others
Posts: 491
Registered: 7-2-2004
Location: Mediterranean
Member Is Offline
Mood: Quantized
|
|
I wouldn't be so worried about that. After all the opening is quite wide, wide enough for gasses to escape quickly.
Btw, if you intend to use a light bulb as a container remove the metal part completely. When I used to leave it the bulb would crack after heating.
Theory guides, experiment decides.
|
|
|
t_Pyro
Hazard to Others
Posts: 120
Registered: 7-2-2004
Location: India
Member Is Offline
Mood: Volatile
|
|
Light bulbs contain an inert gas at low pressure. Since the inert gas (at low temperature) is a bad conductor of heat, the glass capsule does not get
hot too fast. After prolonged use, it does get hot, but by then it has already expanded more or less uniformly to prevent cracking.
Using the glass bulb as lab glassware could be dangerous as the temperature changes involved would be far greater than the glass is designed to
withstand. Drop a drop or two of water on a glowing light bulb, and you'll see...
[Edited on 20-5-2004 by t_Pyro]
|
|
|
Cyrus
Hazard to Others
Posts: 397
Registered: 24-4-2004
Location: Ancient Persia
Member Is Offline
Mood: No Mood
|
|
Maybe I'm missing something but...
Does Na+ migrate through soda lime glass at all temperatures- if so, why can't the electrolysis be done by placing the bulb in a soln. of NaCl-
does H2O also migrate through the glass? Why not use Nafion or Nasicon membranes at room temperature in a soln.?
Sure, Bromic Acid, NASICON is the way to go, but where are you going to get some of that stuff- make your own? The materials aren't too bad but
the process looks pretty involved! Also, you speak as if you had actually done the soda lime glass electrolysis- have you? I would love to hear more
details, as the sodium produced this way sounds like it would be very clean.
I am dissolving the metal end off of a small bulb currenty, any interesting results definitely are going to be posted.
|
|
|
Marvin
National Hazard
Posts: 995
Registered: 13-10-2002
Member Is Offline
Mood: No Mood
|
|
Sodium ions arnt mobile at room temperature in glass, or it wouldnt be an insulator. At 300C or so its noticable, but extremly poor by other
conductors standards.
As far as I am aware, all the sodium ion conductors have to be used at elevated temperature. Many of them were intended for use in applications like
the sodium sulphur battery.
|
|
|
Cyrus
Hazard to Others
Posts: 397
Registered: 24-4-2004
Location: Ancient Persia
Member Is Offline
Mood: No Mood
|
|
| Quote: | Originally posted by Polverone
At one point xoo1246 posted a fascinating patent about producing alkali metals by heating their hydroxides with magnesium in a high-BP hydrocarbon.
|
Sounds very interesting.
I bet polyethylene would work. I should test that.
I just need to go get some Mg (tomorrow)
at $0.25 a lb from a scrap dealer. I think its a powder too. Amazing. I love the Market.
Then I can get around to all those reactions I've been saying I would do. 
All of my previous experiments with sodium have failed.
I did 2 early experiments with NaOH a while back, but I forget what, I just remember that they were hopeless.
Electrolysis 3 - 9v battery, molten NaOH in food can, copper wires. nothing happened- I think the battery was nearly dead by then .
#4- larger 12 v 0.5 a (iirc) power supply,
molten NaOH in food can, Fe wires. Some bubbles, pops, fizzes. The current helped heat the melt, not enough to keep it molten though. Melt turned
green at one wire, brown at the other.
More coming in this sector.
I cleaned out the soda-lime glass lightbulb, and filled the bottom with copper wires. Then I found another smaller lightbulb which had a Cu wire
actually TOUCHING the glass for some reason. Yes!!! Now I don't have to supply vaccuum, heat, and electricity, just heat and electricity!
More coming here.
Sodium thermites
I heated about 1 g NaOH, 1 g Na2CO3, 1 g NaCl, 2.3 g Al in a copper test tube - (got that one for .90$ on one of my recent excursions from Persia to
Home Depot) The Al was not a fine powder, more like finely crumpled shreds of Al - it was from a blender, I have almost no fine Al left.
the apparatus looked like this
_____________________
/ ______________####_- more pipe
/ / __ 90 degree fitting, teflon tape seal
| |
| |- copper test tube
| |
|* | * = thermite
| *|
|* |
|* | # = steel wool
* /
/
After heating for about 0.5 minutes with my torch, there was a loud thump, I lit the H2 gas escaping with the torch, after about 1.5 minutes, the
bottom half of the test tube started glowing very brightly for about 0.5 min, more than the torch could get it alone.
I let it cool, and then looked at the steel wool - should be gobs of Na, right? NOTHING!!! The inside of the copper pipe seemed to have a light white haze on it. The leftover reactants could not be chipped out, so I added
water. Then the fun started. The tube got hot, the mixture fizzed, and lots of H2 came off- enough to light in medium sized fireballs. I did the
reaction again, and the tube gets too hot to hold when water is added.
Then I tried doing the experiment just like Tacho did- lower bowl, upper bowl with water and ice- I heated the lower bowl red hot in places, H2 came
off- enough to make the upper bowl filled with water jump a cm or to into the air , but no violent reaction happened. The lower bowl did not glow bright red except where the torch was. No residues on the upper bowl at all.
Argg!
The only thing I can think of is the Al could be bad- it came from Al foil and the blender. What do you think of the copper condenser apparatus-
it's cheaper and easier to work with than steel pipes.
Sorry for the longevity of the post.
|
|
|
Tacho
National Hazard
Posts: 582
Registered: 5-12-2003
Member Is Offline
Mood: No Mood
|
|
Cyrus,
There is no way the sodium will deposit nicely in the steel wool. The high temperature makes it vaporize. Even the condensed sodium is quite dirty. I
couldn’t even melt it into a single blob.
The only practical uses for this reaction I could find until now are: 1)impress kids igniting the condensed powder with water; 2) to make
methoxide/ethoxide. Even the leftovers react vigorously with alcohols. But be careful, those who try. The leftovers still react violently with water
after they reacted with alcohol.
|
|
|
| Pages:
1
..
3
4
5
6
7
..
13 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
