Chemical Forums
Specialty Chemistry Forums => Citizen Chemist => Topic started by: Aribo on April 24, 2014, 08:16:21 AM
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Hello all!
Been reading a lot on anhydrous AlCl3 production mainly on sm forum and no one seems to have a simple setup for making the aluminium chloride it either had impurities from some of the equip they used to synth. Got a very small amount or nothing at all.
The common setup is as follows DRY HCLg passed over heated aluminium pieces (400degc) resting in a tube the AlCl3 then sublimes out the other side in anhydrous form..
I have drawn up an apparatus to heat the tube to 400 degc + wounded what your thoughts are on it being workable? And the chloride still being dry at the end
As common practice is to heat the tube on a BBQ which I don't have and I would like to perform it inside under my hood as hcl will be involved so a BBQ in bedroom is not the way I want to go. I will upload pictures of the contraption soon as I have figured out how!
On a side boat tried registering for sm but can't? Anyone know why or how I can contact a mod
Thanks and I look forward to your thoughts
Aribo
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To the loose end of the tee will be connected a 600degc heat gun.
Do you think it will heat the internal copper pipe to 400degc or will it loose more heat than the 200degc I can allow to be lost
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1.Hcl is dripped into stirred h2so4
2.Hcl gas is evolved and passed through h2so4 to strip any remaining water
3.the hcl gas passes through the heated tube containing al and reacts
4. Alcl3 sublimes in the 2 litre 2 neck flask
5. Hcl gas is passed through 50% NaOH solution but reliving the hcl gas
6. The NaOH solution also serves as a bubbler and stops air/moisture being drawn into the 2l flask hopefully contains anhydrous alcl3
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I'm not sure this will work.
Also anhydrous AlCl3 is not easy to work with. It is extremely hygroscopic, liberating fumes of HCl on contact with air.
I don't think this preparation should be attempted by an amateur.
Your NaOH trap will rapidly absorb the HCl gas (all the hydrogen produced will bubble through uninterrupted, severe hazard!), creating reduced pressure in your closed system. The result of this will be suck back of your scrubbing solution onto hot aluminium or, if it worked, anhydrous aluminium chloride too.
This will be a violent reaction rapidly liberating hot water vapour, Hydrochloric acid and hydrogen gas.
You would be lucky if you don't seriously hurt yourself attempting this.
I would advise buying it if you really need it.
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Thanks for the response. NaOH trap maybe not the best idea with the current lay out I was thinking to perhaps put a empty trap for solution in between or a drying tube or even a h2s04 trap for moisture. The general method is not untried and has produced alcl3 in varying small yield.. I've also tried but could not heat the al to temp (the reason for my post)
I understand hydrogen is the end result of passing hcl through NaOH also the properties of alcl3 fuming upon contact with air the generation of heat with exposure to water ect ect I am an amateur but certainly not stupid besides everyone's an amateur until they have done something once.
Buying some is an option £16 per 250g on the site we all know and love but why do chemistry if we can just buy? we all may as well hang up our white coats and hand our goggles back.
I wanted to produce a small amount and then try to generate more from it..
On a side note the system would have been flushed of air/moisture
Again thanks for your reply food for thought for sure.
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What do you think will happen when you drop aqueous HCl into conc. sulphuric acid?
I understand hydrogen is the end result of passing hcl through NaOH
No, HCl + NaOH :rarrow: NaCl + H2O
Hydrogen is generated from the following reaction:
2Al + 6HCl :rarrow: 2AlCl3 + 3H2
For for every 267 grams (ca £16) of AlCl3 you produce you will make approximately 30 litres of hydrogen gas. This is enough to cause a serious accident unless everything you are using is spark proof. I can tell you now that your heat gun is not spark proof.
To be fair there is not much about your set up that fills me with confidence. There are much safer, more efficient ways to generate anhydrous HCl to begin with.
After the HCl stage I am afraid you have such serious safety issues that I am unable to offer any more help.
With the greatest of respect and I mean that sincerely because I don't want to put hobbists off conducting propper scientific experiments. Chemists buy chemicals so that they do something more exciting with them, if your goal is to re-invent the wheel then perhaps start with something a little less hazardous.
Anything that involved gaseous acid or base (such as ammonia) is a serious danger to a trained chemist in a fully operational lab with safety equipment and emmergency showers. To put it bluntly, I personally would not conduct this experiment, I am a very experienced chemist but that means I can see every step being a potential hazzard.
If gaseous hydrogen chloride comes into contact with your eyes at a relatively low concentration you will be blinded.
If you are still reading then I guess you may have realised that whether or not you shlould flush the system is a moot point at this stage.
edit: changed "cones into contact" to "comes into contact" for readability
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Thanks for your comments again good for thought, I'm not taking this as a knock I am inexperienced. I wasn't sure this would work that's why I've posted and asked for suggestion and input.
I Appreciate the time you've taken out
Aribo
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@Aribo
If you have not read forum rules please do so = not a reprimand = Just want to make sure we are on the same page.
We have nothing against a reasonable scientific discussion of the properties of drugs and explosives, but we will not help you hurt yourself making them. If you you think your question might cross the line, feel free to send a private message to one of our moderators asking if the questions is acceptable. Note that even if the question is acceptable, discussion may take such a direction we will decide to close the thread. Due to their potential health hazards, we will also not help you prepare your own medicines or cosmetics.
The operative words here are
but we will not help you hurt yourself
Although I support Citizen Science, I want to make sure you are safe.
Since you have seen this on another forum and want to try this, I also appreciate @Archer concern for your safety.
So, just do not go forward with just general Internet knowledge. See if you can read more with in depth discussion (a good University library may be a better source).
Also, wait a bit, to see if there are more responses to your post.
If you have further ideas please post them.
We would rather you NOT actually do the process without some safety input from us if possible.
We in our lab start with Aluminum chloride and do not make it ourselves, so I have no recollected experience. I say recollected since I could have done it eons ago = in class or whatever = but not recent enough for me to remember.
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Thanks for your comments again good for thought, I'm not taking this as a knock I am inexperienced. I wasn't sure this would work that's why I've posted and asked for suggestion and input.
I Appreciate the time you've taken out
Aribo
Let's start at the beginining again, if you could answer my previous question.
What do you think will happen when you drop aqueous HCl into conc. sulphuric acid?
I am happy to help show you the flaws in your setup so that you can do this on a small scale first.
My first reaction with AlCl3 resulted in a rather messy fume hood so it has to be treated with care, don't try to run before you have learned to walk.
You should be able to design something to make small quantities but just throw away your original plan and start with small scale HCl generation and we'll go from there.
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Afternoon Archer.
Hcl.aq Onto H2SO4 will result in Hcl.g and H2SO4.aq
Is this what you ment?
Aribo
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Thanks bill any good books to recommend?
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1) See this http://www.sciencemadness.org/talk/viewthread.php?tid=14224
and
http://www.sciencemadness.org/talk/viewthread.php?tid=14371
2) Dropping conc. H2SO4 on solid NaCl is a better HCl source than dealing with the exotherm of adding conc. HCl to H2SO4. Or dry heat bisulfate and NaCl
Been there, done that. Try not to gas yourself. Don't use Cl2 if your reaction vessel is a copper pipe. Don't bother scrubbing the off-gasses, just do it outside.
What is your issue registering on SM? We have a spammer issue currently and the captcha in use is often hard to read. may take a bunch of tries.
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Also see this. https://www.sciencemadness.org/whisper/viewthread.php?tid=30150
ZnCl2+Al--> Zn + AlCl3.
easy, no gasses, but tube blockage issues. Bet an Ar or N2 stream would help.
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Thanks 408
I have read the first thread which is we're I got the initial design from.. But with a lack of furnace/BBQ need another way to heat the pipe and thought the heatgun would do the trick. maybe some nichrome wire wrapped around the pipe (insulated) could provide the heat?
I'm actually building a spark less fume hood from ply with a neat little sparkless blower, diy carbon filter and epoxy painted for chemical resistance so I hopefully won't have to resort to outside.
Never tried H2SO4 on NaCl will give that a go. I do hear it can foam quite a lot? Or am I confusing this with something else?
Great I'll have a read of the third link when I get a second something new to read!
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I have prepared anhydrous aluminum (III) chloride from chlorine gas and aluminum.(2 Al + 3 Cl2 :rarrow: 2 AlCl3) Because it doesn't give off copious quantities if hydrogen gas, it is a little safer. Chlorine is dangerous to say the least, but so is HCl. The reaction (as one would expect) is self sustaining, and further heating is not required. Everything was done in a SS setup, and the heat generated was used to distill the product.
I hope to try the zinc chloride and aluminum reaction as it will probably be much easier, and certainly safer.
The main reason I used chlorine is because at the time I didn't have much concentrated sulfuric acid, which I would have used to make HCl(g). The chlorine was isolated as such: Ca(OCl)2 + 4 HCl(aq) :rarrow: CaCl2 + 2 H2O + 2 Cl2. BTW, I am very new to this forum, but that doesn't mean I'm a beginner, I'm very active on the Sciencemadness forum, as linked above by 408.
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Because it doesn't give off copious quantities if hydrogen gas, it is a little safer. Chlorine is dangerous to say the least, but so is HCl. 408.
In what way is chlorine gas is safer than hydrogen? If you vent hydrogen appropriately then the risk are very low. Chlorine cannot simply be vented outside.
Sudden accidental inhalation of chlorine is fatal at around 10 ppm the LEL of hydrogen is way in excess of that.
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In what way is chlorine gas is safer than hydrogen? If you vent hydrogen appropriately then the risk are very low. Chlorine cannot simply be vented outside.
Yes, but as I said, I did it mostly because I can isolate chlorine cheaper than I can generate hydrogen chloride. Safety wasn't my biggest concern. I've done many more reactions which used much more toxic gasses, chlorine is jut another. Obviously this wasn't done outside, [Meant inside] it was done in my lab and outside during different stages of the reaction. All of the gasses were also scrubbed, but even this wasn't needed, as the leftover chlorine was "dumped" far away from any people.
Sudden accidental inhalation of chlorine is fatal at around 10 ppm the LEL of hydrogen is way in excess of that.
Care to provide a ref. for that statement?
The first time I made measurable quantities of chlorine, I was stupid, and inhaled some. I'm pretty sure I got more than 10 PPM, but I could be wrong. I did thro up afterwards though...
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Safety wasn't my biggest concern.
Well it should be
The leftover chlorine was "dumped" far away from any people.
Dumping any chemicals without a licence is extremely irresponsible, no matter where it is
Sudden accidental inhalation of chlorine is fatal at around 10 ppm the LEL of hydrogen is way in excess of that.
Care to provide a ref. for that statement?
http://toxnet.nlm.nih.gov/cgi-bin/sis/search/a?dbs+hsdb:@term+@DOCNO+206
B) The OSHA time-weighted average permissible exposure limit
(TWA PEL) is 1 ppm, and the NIOSH immediately dangerous
to life and health (IDLH) level is 10 ppm.
The first time I made measurable quantities of chlorine, I was stupid, and inhaled some. I'm pretty sure I got more than 10 PPM, but I could be wrong. I did thro up afterwards though...
I am very pleased to hear that you did not seriously injure yourself.
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Ok, well what I should have said is safety wasn't something I was exceptionally worried about. I also failed to mention I was wearing a gas mask, which make a big difference.
Dumping any chemicals without a license is extremely irresponsible, no matter where it is.
I made a total of 4 grams of AlCl3. Theoretically, this requires ~.67 liters of chlorine. Because this is the theoretical yield, I generated ~.75 L Cl2 to compensate for inevitable losses. This means ~89% of the chlorine was used up. Which means only 0.0825 L of Cl2 escaped the reaction chamber. Because it was scrubbed out, I highly doubt any sizable amounts of chlorine went into the atmosphere.
Nice link, quite infinitive.
I am very pleased to hear that you did not seriously injure yourself.
Thanks, I guess. I don't know why you are underestimating my safety procedures. This reaction is nothing compared to some of the more elaborate reactions I've done.
[EDIT]All of the reactions I do are with all safety precautions in place, I know what I'm doing.
Mod edit: Offensive language removed. Dan
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Obviously you don't know me but I am being genuine that I am glad that you were not seriously injured by gassing your self with chlorine, presumably you did not have your gas mask on at the time of the incident.
When a chemistry hobbyist is found dead or very seriously injured, the fist question the police ask is regarding the manufacture or attempted manufacture of controlled substances.
When this has been ruled out the coroner or the hospital occasionally seeks counsel as to whether there is a possibility that the injuries sustained were accidental or intentional.
For reasons best known to themselves coroners rarely pre-warn you that there are graphic images in the file.
Maybe if you had seen a persons face who has died from acute exposure to toxic gasses you may understand my concerns over unsafe practices in any lab, whether it be in a kitchen or a fully kitted out state of the art industrial facility.
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I am glad that you were not seriously injured by gassing your self with chlorine, presumably you did not have your gas mask on at the time of the incident.
I appreciate your concern, and you're right, the first time I made isolated chlorine, I wasn't wearing a gas mask. Please understand this was a long time ago. Long before I had much experience.
I was just browsing this forum for the first time, and saw this thread, seeing that nobody had actually experimented with the procedures mentioned, I decided to give my 2 cents worth since I had already done the reaction. I don't understand why you felt like you needed to derail the topic. I know chlorine is toxic. Of course you didn't know that I knew that.
I understand that this board is more for beginners, but I thought you guys would be interested in somebody's personal experience rather than just idea's floating around.
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I thought you guys would be interested in somebody's personal experience
We are.
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I thought you guys would be interested in somebody's personal experience
We are.
Indeed
I have prepared anhydrous aluminum (III) chloride from chlorine gas and aluminum.(2 Al + Cl2 :rarrow: 2 AlCl3) Because it doesn't give off copious quantities if hydrogen gas, it is a little safer. Chlorine is dangerous to say the least, but so is HCl. The reaction (as one would expect) is self sustaining, and further heating is not required. Everything was done in a SS setup, and the heat generated was used to distill the product.
I hope to try the zinc chloride and aluminum reaction as it will probably be much easier, and certainly safer.
The main reason I used chlorine is because at the time I didn't have much concentrated sulfuric acid, which I would have used to make HCl(g). The chlorine was isolated as such: Ca(OCl)2 + 4 HCl(aq) :rarrow: CaCl2 + 2 H2O + 2 Cl2. BTW, I am very new to this forum, but that doesn't mean I'm a beginner, I'm very active on the Sciencemadness forum, as linked above by 408.
I wasn't intending to derail the topic, I intended to highlight to the OP and all of the other amature chemists on here the hazards involved in this process of making chlorine.
Some people will take the information above and just give it a go, having done absolutely no risk assessment.
It is best not to assume experience, knowledge, or a general appreciation of self preservation on Citizen Chemist. This is only my opinion but I am sure that others agree.
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Ok, well thanks for the explanation. Either way, there isn't much more to say about the synthesis. I would enjoy reading other people's accounts on the subject though. I might try a safer method which requires neither chlorine or hydrogen chloride. Direct combination of the elements is by far the cheapest method and is used industrially.
My next attempt will probably be the so-called ''Chlorothermal reactions'', using zinc chloride to oxidize aluminum as mentioned here https://www.sciencemadness.org/whisper/viewthread.php?tid=30150 (https://www.sciencemadness.org/whisper/viewthread.php?tid=30150). I ran out of zinc chloride recently, but it's fairly easy to make or buy http://www.ebay.com/itm/ZINC-CHLORIDE-ZnCl2-800G-ASSAY-99-0-HIGH-GRADE-/201084391150?pt=UK_BOI_Medical_Lab_Equipment_Lab_Supplies_ET&hash=item2ed1904eee (http://www.ebay.com/itm/ZINC-CHLORIDE-ZnCl2-800G-ASSAY-99-0-HIGH-GRADE-/201084391150?pt=UK_BOI_Medical_Lab_Equipment_Lab_Supplies_ET&hash=item2ed1904eee).