Chemical Forums
Chemistry Forums for Students => Organic Chemistry Forum => Topic started by: dudeman on March 20, 2010, 08:16:44 PM
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>:( I cannot find information about how this is made other than a few patents that describe producing it from brines. I was hoping that someone might be able to give me a little insight when it comes to this chemical. You can purchase it online 100 grams for around $18 but what is the fun in that? My idea is to take apart a lithium battery and throw the metal into some naphtha that has had a bunch of dry ice dissolved into it then drop a couple more pieces onto the lithium metal to keep it below the surface... Think it will work? ;D
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Much easier route would be to take the lithium from batteries and react it with aqueous HCl, then add sodium carbonate.
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Somehow I doubt metallic lithium will react with carbon dixoide. Even if, to produce carbonate it will have to reduce part of the CO2 to CO.
Adding some water will change the situation.
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Much easier route would be to take the lithium from batteries and react it with aqueous HCl, then add sodium carbonate.
So the when I get the Lithium Chloride and purify it I could simply add sodium carbonate? Would I need to use a solvent that would dissolve the two powders into solution? Would I need to heat the solution under reflux? Or would the reaction take place on its own?
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Would it work with sodium "bicarbonate"?
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Sorry to post again but I want to say thanks to nj_bartel for the pointer... I found a patent that describes the process thanks to him... Here is the link.
http://www.freepatentsonline.com/3523751.pdf
Thanks for the help...
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My Plan ;D ;D ;D ;D ;D ;D ;D ;D ;D ;D ;D
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Take a 500ml flask and pour in about 250ml of hardware store hcl. Heat this up to 150c for one hour to drive off any water. At this point the temperature can be brought down to 100c. To a beaker that has been heated to 100c the lithium metal is dropped inside. The hot and dry HCL is then poured over the lithium and swashed around in small amounts. When there is no longer an evolution of hydrogen stop adding the HCL. At this point I will allow the HCL to evaporate off completely. I will then add just enough ethyl alcohol to take up the lithium chloride into solution. I will place this onto a magnetic stirring and then slowly begin adding sodium carbonate until it no longer reacts. If the solution becomes to thick to stir more ethyl alcohol will be added. Then 25ml of water is added and allowed to absorb any excess sodium carbonate while the ethyl alcohol is boiled off. The heat will make the lithium carbonate less soluble in water while increasing sodium carbonates solubility. Once the solutions temperature reaches 100C the solids are filtered out and washed with dry ethyl alcohol and allowed to dry.
The dry ethyl alcohol could be substituted with cheap 70% vodka...
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Take a 500ml flask and pour in about 250ml of hardware store hcl. Heat this up to 150c for one hour to drive off any water.
Sigh. How many mistakes one can make in so simple statement.
Please, don't try to do things that you have no idea about.
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Why should I not do this? I know that some HCL will be evaporated out along with any water. All vapor will be expelled through a fume hood. The reason I created that step of my plan was to make sure the lithium didn't react with any water. Will it spontaneously ignite or something when I pour hot acid over it? Please inform me because as you can see I'm really interested in chemistry. I will admit I have not taken any classes but I have done a lot of research.
Plus... How did chemistry come about in the first place? You wouldn't know anything you know if people didn't try things they had no idea about now would you? 8)
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If you heat aqueous hydrochloric acid up to boiling, you're going to drive all the acid off, fast. There shouldn't be any need for heat at all. The oxidation of lithium by HCl will take place at room temp (quite vigorously actually, you should keep the solution cooled if anything). This will yield VERY soluble lithium chloride. To this solution, you add enough sodium carbonate to both neutralize any excess acid and displace chloride to form lithium carbonate and sodium chloride. Lithium carbonate is sparingly soluble in water while sodium chloride is very soluble. Heat the solution at this point to make sure all sodium chloride dissolves, then filter hot to collect the lithium carbonate.
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If you heat aqueous hydrochloric acid up to boiling, you're going to drive all the acid off, fast. There shouldn't be any need for heat at all.
Thanks a lot
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Water also boils at 100 oC. Sure, there's BP elevation, but not 50 oC of it. So there's no way you're heating to 150 oC regardless, which is the other thing I think Borek was driving at.
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Actually concentrated HCl boils below 100 deg C.
You wouldn't know anything you know if people didn't try things they had no idea about now would you?
But we do know now so there is no need to risk your life/health doing things that are obviosuly wrong.
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Why is that, may I ask? Or is that just how the math works out? I've never needed to boil aqueous HCl (I have accidently in a runaway, but that doesn't count), and just assumed it was a normal colligative thing.
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When you get to higher concentrations HCl becomes less dissociated and it is not obvious whether you have solution of HCl in water or water in HCl - and HCl is much more volatile.
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Well just to let you guys know about my acid I will tell you about the time I tried to distill it. The acid never came over. I had a few ml of water come over but that took about a hour. There is a yellow color aswell. My idea to heat to 150c was because my hot plate has to be hotter than the temp I want to get my solution to because it is meant to cook food on. Is there any other way to dry my hcl?
Would it be possible to pump hcl gas into a solvent that has lithium metal suspended in it? Or maybe even pass the hcl gas right over the lithium?
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Wouldn't this work?
1.) lithium metal added to water to make LiOH (lithium hydroxide) and hydrogen gas
2.) bubble CO2 gas into LiOH solution. This should yield Li2CO3 and LiHCO3. Li2CO3 has limited solubility and should start to precipitate.
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Is there any other way to dry my hcl?
No such thing as dry hydrochloric acid.
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HCl in dioxane?
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I know what you mean. Still, I was mostly aiming at the dudeman misconceptions about hydrchloric acid - it is not comparable to sulfuric nor nitric acid that can be prepared as pure ("dry") substances that can be relatively easily used in lab.
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Is there any other way to dry my hcl?
No such thing as dry hydrochloric acid.
Dry hcl (hydrogen chloride) gas IS possible right? So how could I use the dry hcl gas to react with the lithium metal?
I will not give you any more ideas of my own. Please tell me your solution?
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I just learned that hydrogen chloride (the gas that once dissolved in water creates hydrochloric acid) is also soluble in alcohol and ether.
Does lithium metal react with ethyl alcohol?
EDIT!!!
The above information is fail. hydrogen chloride reacts with ethyl alcohol forming ethyl chloride and water...
Would ethyl chloride react with the lithium to form lithium chloride? I'm sure ethyl chloride could be made anhydrous.
This is my main problem... I need a reactant that can be made anhydrous to prevent losses. Any ideas?
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Ok, your setup could be something like
HCl gas generator and "dry" HCl solution prep - roundbottom filled with sodium chloride. add conc. sulfuric acid. Cap roundbottom with a rubber stopper that has a bent glass pipe through it. Put open end of glass pipe into diethyl ether (it's not gonna be completely dry, but close enough). Gently heat roundbottom. Let gas bubble through ether for a few minutes.
Use the HCl in ether solution to prep lithium chloride.
Now, why do you need dry HCl again??
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Ok, your setup could be something like
HCl gas generator and "dry" HCl solution prep - roundbottom filled with sodium chloride. add conc. sulfuric acid. Cap roundbottom with a rubber stopper that has a bent glass pipe through it. Put open end of glass pipe into diethyl ether (it's not gonna be completely dry, but close enough). Gently heat roundbottom. Let gas bubble through ether for a few minutes.
Use the HCl in ether solution to prep lithium chloride.
Now, why do you need dry HCl again??
Well I need it to be dry don't I? Because lithium metal reacts with water to make something different than lithium chloride. If there is any water at all the lithium could react with it which would be a waste of lithium.
So I can get ether to hold the hydrogen chloride? I was put off of the idea when I learned that ethyl alcohol reacts to become ethyl chloride. I will use this method and do some research on it.
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Say it reacts with water. You form Li(OH)2. This is going to react with HCl to form Li(Cl)2
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You form Li(OH)2. This is going to react with HCl to form Li(Cl)2
Oops. More like LiOH & LiCl ;)
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Oui! ;D
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This all sounds over complicated.
Won't this simple synthesis work.
Throw Lithium Into Water.
Bubble CO2 into LiOH solution.
Heat solution to turn bicarbonate to carbonate.
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I think adding to HCl then adding carbonate sounds easier than that :P
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Hey guys! Dudeman here....
So I ordered 250 grams of lithium chloride "brine" from some pyrotechnics shop on ebay and was hoping that you guys could tell me how to purify this stuff... It's already pretty pure. It's a pure white odorless powder that completely dissolves into water.
I already had some sodium carbonate and this also completely dissolves into water.
Ive done a test run so far and it seems to really work! I put a little bit of each into separate beakers and added 10ml of water to each then pour the lithium chloride into the sodium carbonate. It took about five seconds for the reaction to take place. All of a sudden the liquid went white and then it a layer started to form at the bottom. I decanted the liquid and added a bit more water. Decanted then added some acetone. Decanted added more acetone. set aside to dry. The solid precipitate would not dissolve into the acetone. The only test that I have found that I could use to see if this is in fact lithium carbonate is to burn it but I don't have a heat source strong enough to ignite it. Adding hcl to see it bubble off CO2 is pretty pointless since sodium carbonate reacts the same way.
It's late got to go! ;D
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The only test that I have found that I could use to see if this is in fact lithium carbonate is to burn it but I don't have a heat source strong enough to ignite it.
Lithium carbonate doesn't burn, so there is no heat source strong enough to ignite it.
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Decanted then added some acetone.
No.
Filter the precipitated white powder. Rinse with water. Then optionally rinse with acetone. Otherwise you will be precipitating out NaCl into your otherwise-pure Li2CO3.
Suspension in a flame should give the lithium red colour. Addition to HCl should give bubbles. There quick and dirty analysis that does not tell you how pure it is, but that it is Lithium carbonate
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Decanted then added some acetone.
Filter the precipitated white powder. Rinse with water. Then optionally rinse with acetone. Otherwise you will be precipitating out NaCl into your otherwise-pure Li2CO3.
How would this precipitate NaCl? This is confusing to me... (Remember I have no chemistry classes and this is just an awesome hobby)
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If you just decant water, there is much salt containing water still mixed with your precipitated carbonate. If you add acetone to this, you will precipitate out salt from this water as salt is insoluble in acetone. You need to filter the carbonate first, and then rinse with acetone.
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If you just decant water, there is much salt containing water still mixed with your precipitated carbonate. If you add acetone to this, you will precipitate out salt from this water as salt is insoluble in acetone. You need to filter the carbonate first, and then rinse with acetone.
Awesome... Thank you...
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I have edited the thread removing some parts of it, let's stick to synthesis details.
Learn the lesson.
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Borek = Censorship
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Apart from censoring the posts I can also ban users.
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Ok guys I'm back with an update... Thanks for reopening the thread borek.
I have come to believe that the lithium carbonate I have is quite contaminated. I consider the risks and try to understand what could be contaminating it before testing it and think it is relatively safe since there is most likely nothing highly poisonous in it.
The only possible contaminates I can think of would be the reactants. Sodium Carbonate (acidic) and lithium chloride (Small amount of lithium chloride solution had a ph of 4). Both reactants are relatively safe compared to cyanide like one user said earlier on in the thread. I have discovered the product to have a hard time drying out. This might be due to contamination with lithium chloride which LOVES water and basically turns into water if left in the open air. I have also found the product to be slightly irritating when a small amount is rubbed into the skin (not a significant risk under the current circumstances).
Reasons for contamination.
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incorrect proportions of reactants
not enough time given for the reaction to complete
poor conditions of the reaction vessel
(tried washing the lithium carbonate finding it pointless)
Solution to remove contaminants
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Completely dry and powder the contaminated lithium carbonate then pour the powder into a flask. Create a weak solution of lithium chloride in ethyl alcohol (my guess is 10%). Add the solution to the flask. Add a stir bar. Place on magnetic stirrer and let it stir for a couple of hours to completely react with any sodium carbonate. Wash with alcohol 3x to remove any lithium chloride then place the lithium carbonate into a filter and wash once with alcohol to remove any last traces of lithium chloride.
Would this work?
EDIT:
Just to let you guys know. Since some of you are curious. I will be using this substance in some bottle rockets later on down the road. I will upload a picture or two if that is allowed.
No body in their right mind would want to take this substance as a medicine. It's specifically reserved for those who are severely mentally ill and prescribed as a last resort due to the chance of liver and kidney damage. I also believe that it is illegal to sell this substance for ingestion. It's legal to put it in fireworks and stuff though.
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Use the stoichiometric correct amounts of reagents.
Aqueous solutions of each.
Mix and stirr for a few hours
Filter
rinse with water (NOT pointless)
rinse ethanol
dry
make rockets.
Why the lithium salt? Strontium gives red too, and is cheaper.
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Sodium Carbonate (acidic)
if this wasn't a typo, please do some kind of reading so you can understand the chemistry behind your experiment
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Like I said in my last post. How might I remove these contaminants? The mass is to sticky to wash when in the filter 408. The only way I could wash this is to put it back into solution and decant due to the nature of the compound. Its like wet flower only it has the characteristics of corn starch too. To hard to wash.
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Sodium Carbonate (acidic)
if this wasn't a typo, please do some kind of reading so you can understand the chemistry behind your experiment
what I meant was that it is irritating. I got a wiff of some dust from when I opened the bag and wow did my lungs feel a pinch.
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Ah, you lack vacuum filtration...
Decant off supernatant. Add water. stir then allow to settle. Repeat this a bunch of times.
Then filter.
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isnt Li2CO3 dangerous? in a kind a works as a depressant or some.
if its used in pyro and you want the red color, you could try stronium chloride too
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It's an anti depressant. I wonder if this guy has blown himself up yet.
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For the dozens of legit uses people pick one they dislike. Seriously. This is chemistry, not moralizing about what people may or may not do on their own time.
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For the dozens of legit uses people pick one they dislike. Seriously. This is chemistry, not moralizing about what people may or may not do on their own time.
Couldn't agree more.
However, the fact he was considering boiling HCL and dropping in Li is more than a little crazy.
I really want to know what he ended up doing.
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The proposed reaction in my pregrad medicinal chemistry book for production of Li2CO3 is:
Li2SO4 + Na2CO3 -> Li2CO3 + Na2SO4
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Back with an over due update...
I made lithium carbonate... It was cool watching it precipitate... I did not use it for anything and actually just threw it away... I can understand why some of you feel that it is necessary to question my intent since my user name is DUDEMAN...
I learned a lot from this experiment... Thanks to all of those who actually helped.
ONTO THE NEXT TOPIC! ;D ;D
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So what'd you do?