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All 26 posts Subject: Anhydrous HCl in IPA preparation idea Please login to post Down

Bandil
(The Archetypical "Good Guy")
06-02-04 11:36
No 510919
      Anhydrous HCl in IPA preparation idea

Inspired by Post 510698 (Novice: "Try this.", Methods Discourse), I thought of the idea of making anhydrous HCl in IPA using, the following scheme.

Make a suspension of eqimolar amounts of NaCl and CaO in IPA, and drip in equimolar amounts of conc. sulfuric acid. Wouldn't this release HCl in situ into the IPA over time, leaving Ca(OH)₂ and NaHSO₄ as a sludge to be filtered off?

Any ideas, comments?

Thanks, regards
Bandil

Nuke the whales!

starlight
(Hive Bee)
06-02-04 12:13
No 510928
      HCl/ Ca(OH)2

Hmmm.

Although the solubility of calcium hydroxide in alcohol is low, won't the HCl react with the Ca(OH)2 forming CaCl2 which will then react with the IPA?

Pimpo
(Hive Bee)
06-02-04 13:11
No 510939
      gypsum formation?

Starlight might be right. Furthermore I wonder if not finally Ca 2+ would react with SO4 2- to form highly insoluble gypsum. Compare the caustification of soda solutions with Ca(OH)2 which leads to the stronger base NaOH being formed. NaHSO4 might react similar to Na2CO3. NaOH would definately kill the HCl. Of course things in IPA solution might be a lot different from aqueous solution. Just guessing. Why not try the thing on a test tube scale?

Nicodem
(Hive Bee)
06-02-04 14:13
No 510948
User Picture       CaO does not fit in the reaction

Bandil, could you explain what is the purpouse of CaO in your propousal?
Obviously, a sulphuric acid solution in IPA reacts with CaO to yield CaSO4×H2O. It might be worth trying without it and it might just work. H2SO4 is about ten thousants time stronger acid than HCl so it is quite possible that it would drive the HCl in the IPA solution and leave only the NaHSO4 solid. The NaCl should bee finely grinded and in excess to H2SO4 in order to consume as much of it or it as possible. Otherwise it would leave you with too much H2SO4 in the HCl/IPA after decantation.

“The real drug-problem is that we need more and better drugs.” – J. Ott

Novice
(Hive Bee)
06-02-04 14:48
No 510953
      How about ether?

This sounds like a great idea. For me, HCl in ether is of more use, and I wonder if this method could be applied on ether instad of IPA. As I see it, ether should work even better, as most inorganic salts are insoluble in it.

I don't know anything about the solubility of sulphuric acid in ether, however I assume it's not too great, but I don't see why this would be a problem.

Bandil
(The Archetypical "Good Guy")
06-02-04 15:04
No 510954
      sieves

Well the problem with simply mixing sulfuric acid and NaCl in IPA, is that a mole of water is formed for each mole of HCl generated. This water has to be removed somehow. Don't know if the formed NaHSO₄ will soak it up sufficiently?

Otherwise, an alternative approach would be to do the reaction above, and dry the IPA over a proper amount of 3A molecular sieves.

Say for 1 L of 5N IPA, the following would be required:

1 L IPA
5 moles NaCl
5 moles H₂SO₄

Let it react, and decant the IPA, rinsing the sludge with a little more fresh IPA, to get a total volume of 1 L.

5 moles of water should be present here. This would require(assuming 20% wt% capacity of the sieves):

18g/mole * 5mole = 90 / 0.2 = 450 g's sieves (500 g's to be sure).

Sure is a lot of sieves to use, but the can of course be reused over and over to generate unlimited supplies of cheap dry HCl / IPA...

Comments?

Regards
Bandil

Nuke the whales!

Novice
(Hive Bee)
06-02-04 15:10
No 510956
      No water is formed...

Bandil, no water is formed in this reaction, so there's no need to dry it - which makes it even more simple :-)

H₂SO₄ + NaCl -> NaHSO₄ + HCl

Bandil
(The Archetypical "Good Guy")
06-02-04 16:07
No 510970
      BRAINFART

As the subject line says - sorry about that...

Hmmm... sounds like its worth a try wink

Regards
Bandil

Nuke the whales!

Barium
(Heavyweight Chempion(eer))
06-02-04 21:45
No 511043
      How about using calcium chloride instead?

How about using calcium chloride instead?

CaCl₂ + H₂SO₄ --> CaSO₄(s) + 2HCl

Severe Aztecoholic and President of Sooty's fanclub - Sooty for President!!

Antoncho
(Official Hive Translator)
06-03-04 02:05
No 511125
      Filtering

Filtering's gonna bee a bitch.

OTOH, NaCl is too poorly soluble in IPA to provide for a complete conversion of H2SO4. IMO.

Yet another objection - NaHSO4 is much more alcohol-soluble, and it will also act as an excellent acid in terms of amines' acidification, won't it?

Maybee, better use straight NaHSO4 in IPA? laugh

P.S. After all this using CaCl2 beegins to seem like the best option smile

Bond_DoubleBond
(Hive Bee)
06-03-04 02:59
No 511140
      negative on CaCl2

cacl2 doesn't work with alcohols

hest
(Hive Adickt)
06-03-04 05:07
No 511153
      gassingg

If I was old and grumpy I would say that the usual way by just gassing is much more easy wink

Bandil
(The Archetypical "Good Guy")
06-03-04 09:25
No 511186
      Bond_DoubleBond> Found the chart on ...

Bond_DoubleBond>

Found the chart (https://www.rhodium.ws/chemistry/equipment/dryingagent.html) on rhodium's side, that states that they are not compatible. But isn't this simply if they contain amines, which will be complexed?

Besides that the CaCl₂, will be converted to CaSO₄ the instant the sulfuric acid is added.

On the other hand, one could premix the acid and alcohol, and then add the finely powdered CaCl₂ carefully, to ensure complete conversion.

Hest> Gassing is cool in a real lab with fumehood etc. Gassing is not fun when confined to less fancy locations wink So there: You are and old grumpy gassing man tongue

Enjoy

Regards
Bandil

Nuke the whales!

Rhodium
(Chief Bee)
06-03-04 12:59
No 511211
User Picture       alcohols of crystallization

Calcium chloride forms "alcohols of crystallization" just like it forms hydrates. Anything with a lone pair will complex with Ca²⁺

^{The Hive - Clandestine Chemists Without Borders}

Bandil
(The Archetypical "Good Guy")
06-03-04 13:10
No 511213
      Rhodium> Does this mean that the Calcium...

Rhodium>
Does this mean that the Calcium salts will be soluble in alcohol (IPA in this case)? Or will it simply imply that some of the alcohol will be trapped in the CaSO₄? In that case a little extra IPA should take care of the problem.

So, what salt would you suggest dr. chief? And please don't suggest gassing, as its the whole point to avoid this wink

There has to be an easy easy way of getting HCl / IPA without "Camp Auswitch" with your own health wink

Regards
Bandil

Nuke the whales!

Rhodium
(Chief Bee)
06-03-04 14:03
No 511219
User Picture       Magic desiccant

Does this mean that the Calcium salts will be soluble in alcohol (IPA in this case)? Or will it simply imply that some of the alcohol will be trapped in the CaSO4?

Mainly the latter, but a slight solubility of some calcium isopropylate chlorides cannot be ruled out.

What you need is a desiccant which is neutral or acidic and which does not react with or dissolve in alcohols. I don't know if anything besides molecular sieves would fit that description.

^{The Hive - Clandestine Chemists Without Borders}

xxxxx
(Hive Bee)
06-03-04 16:41
No 511245
      convienient prep ?

i would like to suggest the following procedure. take a 500 ml jar of 34% hcl and a 500 ml jar of ipa and place them together in a 4000 ml jar with a lid. after a day or two the hcl vapor should go into the ipa.

Rhodium
(Chief Bee)
06-03-04 17:03
No 511249
User Picture       At least respect the Laws of Thermodynamics...

Most definitely not. Water has a considerable higher affinity for hydrogen chloride than any alcohol has.

^{The Hive - Clandestine Chemists Without Borders}

Barium
(Heavyweight Chempion(eer))
06-04-04 00:54
No 511325
      One very convinient way of preparing alcoholic

One very convinient way of preparing alcoholic solutions of HCl is to add e.g. acetyl chloride to IPA. This gives of course a mixture of IPA and isopropyl acetate if excess IPA is used, but the ester will not interfere with the formation of most hydrochlorides. In most cases it will even aid the crystallisation.

Severe Aztecoholic and President of Sooty's fanclub - Sooty for President!!

hest
(Hive Adickt)
06-04-04 05:45
No 511356
      Ether

Why not use ether ? mixing dry ether (or THF) with HCl(aq) and then dry out the wather ?. I'v done it with H2O2 and it works fine. Actual ill give it a try now.

hest
(Hive Adickt)
06-04-04 06:57
No 511366
      THF

100mL THF and 50mL HCl was mixed (exoterm) for 1 min, then 50-70g MgSO4 was added (more exoterm), and the mixture filtered.
Titration of the THF indikated an 2.4M HCl in THF solution.
Iff you don't have a fumehood cool with ice :-)
Ill give ether a shot later on.

Bandil
(The Archetypical "Good Guy")
06-04-04 07:00
No 511367
      Kisses for you

Kisses for you Hest cool

Seems like a very easy procedure. Do you know how much HCl ether can hold?

Regards
Bandil

Nuke the whales!

hest
(Hive Adickt)
06-04-04 10:12
No 511407
      Ether

When I gass ether I'll usual end up with an 5-6M so Iguess that's the limit.

hest
(Hive Adickt)
06-04-04 11:22
No 511424
      HCl in Ether

100mL diethylether was stirred with 50mL 12MHCl (exoterm) for 1 min, the ether was seprated from the HCl(aq), dryed with Mgso4. The MgSO4 was filtereed off and 10 mL of the ether was mixed with wather and titrated. yeald was an 0,22M HCl in ether solution.
Guess this could bee repeated to increase the ether-consentration (cooling and longer reacton-time might help too)

Nicodem
(Hive Bee)
06-04-04 11:29
No 511427
User Picture       Add some CaCl2

Adding some anhydrous CaCl2 into the HCl(aq)/Ether mixture would force much more HCl into the ether phase. Considerably more as the water phase would get way oversaturated with HCl. Don't exagerate on the amount of CaCl2 though, or you will gas the whole lab with HCl fumes. Just a sugestion to improve the otherwise nice and practical idea. smile

“The real drug-problem is that we need more and better drugs.” – J. Ott

hest
(Hive Adickt)
06-05-04 14:23
No 511618
      gassing

The ether from the post above was treated with 12M HCl for 12H, seperated, dryet and titrated, still 0.22M.
So if we have 15g(71mmol) mescaline disolved into 100mL ether we have to add 322mL 0,22M hcl in ether to make the hydrochloride. Thats not good enough.

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	All 26 posts		Subject: Anhydrous HCl in IPA preparation idea		Please login to post		Down


		Bandil (The Archetypical "Good Guy") 06-02-04 11:36 No 510919				Anhydrous HCl in IPA preparation idea
						Inspired by Post 510698 (Novice: "Try this.", Methods Discourse), I thought of the idea of making anhydrous HCl in IPA using, the following scheme. Make a suspension of eqimolar amounts of NaCl and CaO in IPA, and drip in equimolar amounts of conc. sulfuric acid. Wouldn't this release HCl in situ into the IPA over time, leaving Ca(OH)₂ and NaHSO₄ as a sludge to be filtered off? Any ideas, comments? Thanks, regards Bandil Nuke the whales!



		starlight (Hive Bee) 06-02-04 12:13 No 510928				HCl/ Ca(OH)2
						Hmmm. Although the solubility of calcium hydroxide in alcohol is low, won't the HCl react with the Ca(OH)2 forming CaCl2 which will then react with the IPA?



		Pimpo (Hive Bee) 06-02-04 13:11 No 510939				gypsum formation?
						Starlight might be right. Furthermore I wonder if not finally Ca 2+ would react with SO4 2- to form highly insoluble gypsum. Compare the caustification of soda solutions with Ca(OH)2 which leads to the stronger base NaOH being formed. NaHSO4 might react similar to Na2CO3. NaOH would definately kill the HCl. Of course things in IPA solution might be a lot different from aqueous solution. Just guessing. Why not try the thing on a test tube scale?



		Nicodem (Hive Bee) 06-02-04 14:13 No 510948				CaO does not fit in the reaction
						Bandil, could you explain what is the purpouse of CaO in your propousal? Obviously, a sulphuric acid solution in IPA reacts with CaO to yield CaSO4×H2O. It might be worth trying without it and it might just work. H2SO4 is about ten thousants time stronger acid than HCl so it is quite possible that it would drive the HCl in the IPA solution and leave only the NaHSO4 solid. The NaCl should bee finely grinded and in excess to H2SO4 in order to consume as much of it or it as possible. Otherwise it would leave you with too much H2SO4 in the HCl/IPA after decantation. “The real drug-problem is that we need more and better drugs.” – J. Ott



		Novice (Hive Bee) 06-02-04 14:48 No 510953				How about ether?
						This sounds like a great idea. For me, HCl in ether is of more use, and I wonder if this method could be applied on ether instad of IPA. As I see it, ether should work even better, as most inorganic salts are insoluble in it. I don't know anything about the solubility of sulphuric acid in ether, however I assume it's not too great, but I don't see why this would be a problem.



		Bandil (The Archetypical "Good Guy") 06-02-04 15:04 No 510954				sieves
						Well the problem with simply mixing sulfuric acid and NaCl in IPA, is that a mole of water is formed for each mole of HCl generated. This water has to be removed somehow. Don't know if the formed NaHSO₄ will soak it up sufficiently? Otherwise, an alternative approach would be to do the reaction above, and dry the IPA over a proper amount of 3A molecular sieves. Say for 1 L of 5N IPA, the following would be required: 1 L IPA 5 moles NaCl 5 moles H₂SO₄ Let it react, and decant the IPA, rinsing the sludge with a little more fresh IPA, to get a total volume of 1 L. 5 moles of water should be present here. This would require(assuming 20% wt% capacity of the sieves): 18g/mole * 5mole = 90 / 0.2 = 450 g's sieves (500 g's to be sure). Sure is a lot of sieves to use, but the can of course be reused over and over to generate unlimited supplies of cheap dry HCl / IPA... Comments? Regards Bandil Nuke the whales!



		Novice (Hive Bee) 06-02-04 15:10 No 510956				No water is formed...
						Bandil, no water is formed in this reaction, so there's no need to dry it - which makes it even more simple :-) H₂SO₄ + NaCl -> NaHSO₄ + HCl



		Bandil (The Archetypical "Good Guy") 06-02-04 16:07 No 510970				BRAINFART
						As the subject line says - sorry about that... Hmmm... sounds like its worth a try Regards Bandil Nuke the whales!



		Barium (Heavyweight Chempion(eer)) 06-02-04 21:45 No 511043				How about using calcium chloride instead?
						How about using calcium chloride instead? CaCl₂ + H₂SO₄ --> CaSO₄(s) + 2HCl Severe Aztecoholic and President of Sooty's fanclub - Sooty for President!!



		Antoncho (Official Hive Translator) 06-03-04 02:05 No 511125				Filtering
						Filtering's gonna bee a bitch. OTOH, NaCl is too poorly soluble in IPA to provide for a complete conversion of H2SO4. IMO. Yet another objection - NaHSO4 is much more alcohol-soluble, and it will also act as an excellent acid in terms of amines' acidification, won't it? Maybee, better use straight NaHSO4 in IPA? P.S. After all this using CaCl2 beegins to seem like the best option



		Bond_DoubleBond (Hive Bee) 06-03-04 02:59 No 511140				negative on CaCl2
						cacl2 doesn't work with alcohols



		hest (Hive Adickt) 06-03-04 05:07 No 511153				gassingg
						If I was old and grumpy I would say that the usual way by just gassing is much more easy



		Bandil (The Archetypical "Good Guy") 06-03-04 09:25 No 511186				Bond_DoubleBond> Found the chart on ...
						Bond_DoubleBond> Found the chart (https://www.rhodium.ws/chemistry/equipment/dryingagent.html) on rhodium's side, that states that they are not compatible. But isn't this simply if they contain amines, which will be complexed? Besides that the CaCl₂, will be converted to CaSO₄ the instant the sulfuric acid is added. On the other hand, one could premix the acid and alcohol, and then add the finely powdered CaCl₂ carefully, to ensure complete conversion. Hest> Gassing is cool in a real lab with fumehood etc. Gassing is not fun when confined to less fancy locations So there: You are and old grumpy gassing man Enjoy Regards Bandil Nuke the whales!



		Rhodium (Chief Bee) 06-03-04 12:59 No 511211				alcohols of crystallization
						Calcium chloride forms "alcohols of crystallization" just like it forms hydrates. Anything with a lone pair will complex with Ca²⁺ ^{The Hive - Clandestine Chemists Without Borders}



		Bandil (The Archetypical "Good Guy") 06-03-04 13:10 No 511213				Rhodium> Does this mean that the Calcium...
						Rhodium> Does this mean that the Calcium salts will be soluble in alcohol (IPA in this case)? Or will it simply imply that some of the alcohol will be trapped in the CaSO₄? In that case a little extra IPA should take care of the problem. So, what salt would you suggest dr. chief? And please don't suggest gassing, as its the whole point to avoid this There has to be an easy easy way of getting HCl / IPA without "Camp Auswitch" with your own health Regards Bandil Nuke the whales!



		Rhodium (Chief Bee) 06-03-04 14:03 No 511219				Magic desiccant
						Does this mean that the Calcium salts will be soluble in alcohol (IPA in this case)? Or will it simply imply that some of the alcohol will be trapped in the CaSO4? Mainly the latter, but a slight solubility of some calcium isopropylate chlorides cannot be ruled out. What you need is a desiccant which is neutral or acidic and which does not react with or dissolve in alcohols. I don't know if anything besides molecular sieves would fit that description. ^{The Hive - Clandestine Chemists Without Borders}



		xxxxx (Hive Bee) 06-03-04 16:41 No 511245				convienient prep ?
						i would like to suggest the following procedure. take a 500 ml jar of 34% hcl and a 500 ml jar of ipa and place them together in a 4000 ml jar with a lid. after a day or two the hcl vapor should go into the ipa.



		Rhodium (Chief Bee) 06-03-04 17:03 No 511249				At least respect the Laws of Thermodynamics...
						Most definitely not. Water has a considerable higher affinity for hydrogen chloride than any alcohol has. ^{The Hive - Clandestine Chemists Without Borders}



		Barium (Heavyweight Chempion(eer)) 06-04-04 00:54 No 511325				One very convinient way of preparing alcoholic
						One very convinient way of preparing alcoholic solutions of HCl is to add e.g. acetyl chloride to IPA. This gives of course a mixture of IPA and isopropyl acetate if excess IPA is used, but the ester will not interfere with the formation of most hydrochlorides. In most cases it will even aid the crystallisation. Severe Aztecoholic and President of Sooty's fanclub - Sooty for President!!



		hest (Hive Adickt) 06-04-04 05:45 No 511356				Ether
						Why not use ether ? mixing dry ether (or THF) with HCl(aq) and then dry out the wather ?. I'v done it with H2O2 and it works fine. Actual ill give it a try now.



		hest (Hive Adickt) 06-04-04 06:57 No 511366				THF
						100mL THF and 50mL HCl was mixed (exoterm) for 1 min, then 50-70g MgSO4 was added (more exoterm), and the mixture filtered. Titration of the THF indikated an 2.4M HCl in THF solution. Iff you don't have a fumehood cool with ice :-) Ill give ether a shot later on.



		Bandil (The Archetypical "Good Guy") 06-04-04 07:00 No 511367				Kisses for you
						Kisses for you Hest Seems like a very easy procedure. Do you know how much HCl ether can hold? Regards Bandil Nuke the whales!



		hest (Hive Adickt) 06-04-04 10:12 No 511407				Ether
						When I gass ether I'll usual end up with an 5-6M so Iguess that's the limit.



		hest (Hive Adickt) 06-04-04 11:22 No 511424				HCl in Ether
						100mL diethylether was stirred with 50mL 12MHCl (exoterm) for 1 min, the ether was seprated from the HCl(aq), dryed with Mgso4. The MgSO4 was filtereed off and 10 mL of the ether was mixed with wather and titrated. yeald was an 0,22M HCl in ether solution. Guess this could bee repeated to increase the ether-consentration (cooling and longer reacton-time might help too)



		Nicodem (Hive Bee) 06-04-04 11:29 No 511427				Add some CaCl2
						Adding some anhydrous CaCl2 into the HCl(aq)/Ether mixture would force much more HCl into the ether phase. Considerably more as the water phase would get way oversaturated with HCl. Don't exagerate on the amount of CaCl2 though, or you will gas the whole lab with HCl fumes. Just a sugestion to improve the otherwise nice and practical idea. “The real drug-problem is that we need more and better drugs.” – J. Ott



		hest (Hive Adickt) 06-05-04 14:23 No 511618				gassing
						The ether from the post above was treated with 12M HCl for 12H, seperated, dryet and titrated, still 0.22M. So if we have 15g(71mmol) mescaline disolved into 100mL ether we have to add 322mL 0,22M hcl in ether to make the hydrochloride. Thats not good enough.

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