organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
Simple CCl4 preparation?
CS2 + Cl2 ==> CCl4 + S2Cl2
With Iodine as the catalyst.
I came across this prep for CCl4 and was wondering if anyone has tried and had any luck?
After searching, there does not seem to be a whole lot preps that are not very complicated.
This seems like something I would like to try. Ill post my results soon.
[Edited on 7-4-2016 by organicchemist25]
|
|
|
macckone
Dispenser of practical lab wisdom
Posts: 2168
Registered: 1-3-2013
Location: Over a mile high
Member Is Offline
Mood: Electrical
|
|
Easier method, prepare chloroform, then chlorinate with chlorine in uv light as a gas phase reaction.
also easier, gas phase chlorination of methane. This one is very exothermic. And again a uv initiator works best.
|
|
|
urenthesage
Hazard to Self
Posts: 77
Registered: 21-2-2016
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by organicchemist25  | CS2 + Cl2 ==> CCl4 + S2Cl2
With Iodine as the catalyst.
I came across this prep for CCl4 and was wondering if anyone has tried and had any luck?
After searching, there does not seem to be a whole lot preps that are not very complicated.
This seems like something I would like to try. Ill post my results soon.
[Edited on 7-4-2016 by organicchemist25] |
Careful with that preparation. A recent UN treaty, which your country signed (unless you live in iran, sudan, or north korea) and has probably
ratified puts s2cl2 as a precursor chemical in the manufacture of chemical weapons. They probably wont give a shit but the potential for arrest is
still there.
|
|
|
woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
| Quote: Originally posted by urenthesage | | Careful with that preparation. A recent UN treaty, which your country signed (unless you live in iran, sudan, or north korea) and has probably
ratified puts s2cl2 as a precursor chemical in the manufacture of chemical weapons. They probably wont give a shit but the potential for arrest is
still there. |
Don't make people afraid with this kind of posts. S2Cl2, SOCl2 and quite a few other chems like PCl3, POCl3, PCl5 are so-called CWC-precursors, but if
you make a few tens of grams of these at home, nobody will care. CWC-precursors may not be sold or exported without the necessary paperwork, but that
kind of regulations only is relevant for transfers of tonne-quantities. If you have 100 gram or so of one of these compounds, then you simply cannot
make chemical weapons. Besides that, making a real weapon from precursors is not easy at all and requires considerable engineering effort. Of course,
you might be able to make something which kills yourself or your home-mates, but that can also be done with other things, such as blowing up your
house with the butane gas from a camping gas heater.
There may be many other reasons of not doing this synthesis, such as the danger of fire, the danger of poisoning yourself or the risk of explosion of
air/CS2 mixes, but the fact that S2Cl2 may be on some CWC-precursor list definitely is not one of them.
[Edited on 7-4-16 by woelen]
|
|
|
Dr.Bob
International Hazard
Posts: 2748
Registered: 26-1-2011
Location: USA - NC
Member Is Offline
Mood: No Mood
|
|
The bigger problem is that CS2 is often much harder to get than CCl4. And for many cases it is not a very good solvent. I would certainly try to
chlorinate CHCl3 before doing a chlorination of CS2, that is likely very messy, and SF4 might be made, and it is quite toxic, I don't care about CWC
rules at home, but don't want to kill myself, and those types of reactions are not easy. Woelen is right that regulations are not the problem, but
dealing with CS2, Cl2, and S2Cl2 is not very easy at home. If you really need CCl4, I would try to buy it, it is not that hard to find small
quantities, but I would try to use perchloroethylene, chloroform, or other more obtainable solvents if possible.
|
|
|
organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by macckone | Easier method, prepare chloroform, then chlorinate with chlorine in uv light as a gas phase reaction.
also easier, gas phase chlorination of methane. This one is very exothermic. And again a uv initiator works best. |
Would you happen to know what wattage and best bulb to use, as Ive heard some filter out a lot of the UV.
Thanks
|
|
|
organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by woelen | | Quote: Originally posted by urenthesage | | Careful with that preparation. A recent UN treaty, which your country signed (unless you live in iran, sudan, or north korea) and has probably
ratified puts s2cl2 as a precursor chemical in the manufacture of chemical weapons. They probably wont give a shit but the potential for arrest is
still there. |
Don't make people afraid with this kind of posts. S2Cl2, SOCl2 and quite a few other chems like PCl3, POCl3, PCl5 are so-called CWC-precursors, but if
you make a few tens of grams of these at home, nobody will care. CWC-precursors may not be sold or exported without the necessary paperwork, but that
kind of regulations only is relevant for transfers of tonne-quantities. If you have 100 gram or so of one of these compounds, then you simply cannot
make chemical weapons. Besides that, making a real weapon from precursors is not easy at all and requires considerable engineering effort. Of course,
you might be able to make something which kills yourself or your home-mates, but that can also be done with other things, such as blowing up your
house with the butane gas from a camping gas heater.
There may be many other reasons of not doing this synthesis, such as the danger of fire, the danger of poisoning yourself or the risk of explosion of
air/CS2 mixes, but the fact that S2Cl2 may be on some CWC-precursor list definitely is not one of them.
[Edited on 7-4-16 by woelen] |
I wasn't sure, but I figured that CS2 may be hard to obtain as I havent really heard of that specific compound, at least not that I can recall right
off.
Thanks...Ill try the UV chlorination.
|
|
|
organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by Dr.Bob | | The bigger problem is that CS2 is often much harder to get than CCl4. And for many cases it is not a very good solvent. I would certainly try to
chlorinate CHCl3 before doing a chlorination of CS2, that is likely very messy, and SF4 might be made, and it is quite toxic, I don't care about CWC
rules at home, but don't want to kill myself, and those types of reactions are not easy. Woelen is right that regulations are not the problem, but
dealing with CS2, Cl2, and S2Cl2 is not very easy at home. If you really need CCl4, I would try to buy it, it is not that hard to find small
quantities, but I would try to use perchloroethylene, chloroform, or other more obtainable solvents if possible. |
I have thought about buying it and it is really just a solvent I wanted to add to the lab. I have seen it often in literature, but not in immediate
need of it. I also like to try and make solvents or reagents if possible. Its just more educational and more fun than just buying it. But, ill buy a
little if I fail or Ill try again. 
Thanks
|
|
|
organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
All replies were valid and helpful, which is why I love this community! Thanks again
|
|
|
Metacelsus
International Hazard
Posts: 2539
Registered: 26-12-2012
Location: Boston, MA
Member Is Offline
Mood: Double, double, toil and trouble
|
|
| Quote: Originally posted by Dr.Bob | | I would certainly try to chlorinate CHCl3 before doing a chlorination of CS2, that is likely very messy, and SF4 might be made, and it is quite toxic,
I don't care about CWC rules at home, but don't want to kill myself, and those types of reactions are not easy. |
Wait - how would SF4 be made? Where would the fluorine come from?
|
|
|
Dr.Bob
International Hazard
Posts: 2748
Registered: 26-1-2011
Location: USA - NC
Member Is Offline
Mood: No Mood
|
|
Sorry, I meant SCl4, which is also toxic. SF4 is a highly toxic intermediate in fluorine chemistry, just was looking at some fluorine chemistry
recently so I had it on the mind.
|
|
|
urenthesage
Hazard to Self
Posts: 77
Registered: 21-2-2016
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by woelen | | Quote: Originally posted by urenthesage | | Careful with that preparation. A recent UN treaty, which your country signed (unless you live in iran, sudan, or north korea) and has probably
ratified puts s2cl2 as a precursor chemical in the manufacture of chemical weapons. They probably wont give a shit but the potential for arrest is
still there. |
Don't make people afraid with this kind of posts. S2Cl2, SOCl2 and quite a few other chems like PCl3, POCl3, PCl5 are so-called CWC-precursors, but if
you make a few tens of grams of these at home, nobody will care. CWC-precursors may not be sold or exported without the necessary paperwork, but that
kind of regulations only is relevant for transfers of tonne-quantities. If you have 100 gram or so of one of these compounds, then you simply cannot
make chemical weapons. Besides that, making a real weapon from precursors is not easy at all and requires considerable engineering effort. Of course,
you might be able to make something which kills yourself or your home-mates, but that can also be done with other things, such as blowing up your
house with the butane gas from a camping gas heater.
There may be many other reasons of not doing this synthesis, such as the danger of fire, the danger of poisoning yourself or the risk of explosion of
air/CS2 mixes, but the fact that S2Cl2 may be on some CWC-precursor list definitely is not one of them.
[Edited on 7-4-16 by woelen] |
Im not trying to scare anyone sir. Im simply stating that if your govt gets a wild butthair up its ass they CAN arrest you, that doesnt mean they will
but the possibility exists. You wouldnt believe what is on those lists, simple stuff like acetic anhydride can technically get you jail time. Im not
suggesting that you dont do these chemicals, I plan on making quite a few that are on this list, and I already have a few of them.
|
|
|
MrMario
Harmless
Posts: 46
Registered: 2-2-2016
Member Is Offline
Mood: No Mood
|
|
May I ask what makes CCl4 more prefered as DCM or Chloroform? It seems that it has a high toxicity and is probably harder to get than DCM and
Chloroform.
|
|
|
macckone
Dispenser of practical lab wisdom
Posts: 2168
Registered: 1-3-2013
Location: Over a mile high
Member Is Offline
Mood: Electrical
|
|
Carbon tetrachloride is a truly nonpolar solvent. The others are still somewhat polar. Although I have not run across reactions where this matters,
it is certainly conceivable. Also with very agressive chlorinating agents, the fully chlorinated compund might be preferred.
|
|
|
Electra
Hazard to Others
Posts: 179
Registered: 11-12-2013
Member Is Offline
Mood: No Mood
|
|
To add to macckone's method above. Instead of working directly with chlorine gas/liquid, you should be able to use a pool chlorinator like TCCA.
Though I would suggest either a dimethylhydantoin or Succinimide derivative since the byproduct is water soluble, whereas cyanuric acid from TCCA is
not.
|
|
|
CuReUS
National Hazard
Posts: 928
Registered: 9-9-2014
Member Is Offline
Mood: No Mood
|
|
here are two methods :
from phosgene  - http://www.google.co.in/patents/US2892875 (yield=86%)
from toluene (yield=95%) or m-xylene (yield=97%) - "Journal of applied chemistry of the USSR, , vol. 57, # 2 pt 2 p. 321 - 324"
|
|
|
Daffodile
Hazard to Others
Posts: 167
Registered: 7-3-2016
Location: Highways of Valhalla
Member Is Offline
Mood: Riding eternal
|
|
Can't you just buy Carbon Tetrachloride? Its used to clean spots on metal before soldering/ inlaying. I haven't seen a bottle lying around the school
workshop or anything but the handbook says to just ask the teacher for some.
|
|
|
macckone
Dispenser of practical lab wisdom
Posts: 2168
Registered: 1-3-2013
Location: Over a mile high
Member Is Offline
Mood: Electrical
|
|
Carbon tetrachloride is not as available as it was 30 years ago. I haven't seen it in a consumer products since I was a kid.
|
|
|
solitanze
Harmless
Posts: 26
Registered: 4-2-2016
Member Is Offline
Mood: No Mood
|
|
This may help: http://www.sciencemadness.org/talk/viewthread.php?tid=10300
|
|
|
organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
Thanks for the link. Sorry for late reply. I always forget to check the receive email on reply box.
|
|
|
Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline
Mood: Chemistry: the subtle science.
|
|
CCl4 can be made in high yield and good purity at home this way, but it is not simple or cheap:
https://www.sciencemadness.org/whisper/viewthread.php?tid=14...
The single most important condition for a successful synthesis is good mixing - Nicodem
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
