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All 17 posts Subject: NH3 - anhydrous Please login to post Down

Organikum
(Wonderful Personality)
03-20-04 19:59
No 496351
      NH3 - anhydrous
(Rated as: good idea!)

Sometimes the chemist would love to have some ammonia gas in its anhydrous form available in his laboratory without being forced to buy a gascylinder full of this compound which has gotten an somehow evil smell (it always was bad smelling of course) because of its inflationary use in the manufacture of methamphetamine from pseudoephedrine containing pills.

How to produce this compound quick and easy and - anhydrous?
The best method known to me by now was posted by lugh long time ago and used CaO and NH4Cl to free the ammonia from its salt. Drawback here is that water is formed in the reaction and an additional drying tower with CaO/NaOh is required for to get the ammonia almost anhydrous, another drawback is that CaO is not everywhere easily available, probably because of its properties in dissoving cadavers quick and complete.

As I got interested in this ammonia lately - NO! Not for reductive amination purposes, but for use as fertilizer thats understood - I searched a lil´ bit and found this:

3CH4N2O + heat = C3H3N3O3 + 3NH3
Urea + heat = cyanuric acid + ammonia

Preparation of cyanuric acid:
...More practically by heating urea until the evolution of ammonia ceases and the mass becomes solid again; ....

REMARK: Urea melts at about 135°C. Cyanuric acid at about 330°C. I the reaction biuret is formed as an intermediate which melts/decomposes at about 190°C, so the favorable reaction temperature is between 200°C and 300°C. Even higher temperatures will even decompose the cyanuric acid to cyanic acid and CO2, whereby the cyanic acid will form NH3 with any water present, but its easier to stop at the cyanuric acid stage which is a valuable compound for its own in my eyes. Higher temperatures wont make any problems though.

Ref:
- Wöhlers Outline of Organic Chemistry, 1873, page 216ff.
- MERCK Index 2002.

Calculated yields (approx.): 410ml (~280gram) anhydrous ammonia (liquid@-34°C) from 1kg dry urea.
Not sooo bad I want to say, for urea is dirtcheap, everywhere available and the procedure is not what I would call rocketscience. laugh

The procedure was tested and works.

Shareholder of Paranoid Fucks inc.

thermalpressure
(Stranger)
08-09-04 18:24
No 524449
      Generator setup uses

May I ask what type of setup is to be used. Is a drying tower still necessary. What about a precooler would a regular spiral condenser suffice as a precooler.

Organikum
(Wonderful Personality)
08-09-04 18:43
No 524451
      As told this produces ammonia without water...

As told this produces ammonia without water (dry/dried urea is understood - dry it just below the docomposition temperature... ).

As told the ammonia will be pretty hot though free from water. A iron or SS tube-spiral through icewater will suffice as precooler - a standard spriral glasscooler fed with icewater will suffice if the amount of ammonia is not to large. No copper, no brass but plain old iron/mild steel is perfectly ok here.

Your question is not to answer universally as cooling depends on the amounts processed, heat transfer capability, temperature difference...and, and, and...

hope this helps nevertheless.

so near, so far......

quantum
(Hive Bee)
08-16-04 03:19
No 525632
      try this

put high ammonia containing fert with sodium hydroxide then heat too easy and fucking cheap

e3500 console login: root
bash-2.05#

Organikum
(Wonderful Personality)
08-16-04 05:56
No 525691
      Hmmmmm....Re: put high ammonia containing fert

Hmmmmm....
put high ammonia containing fert with sodium hydroxide then heat too easy and fucking cheap

I dont know what this fertilizer exactly contains. Heating ammonium nitrate left a rather big hole in Oklahoma City lately AFAIK.

If the fertilizer is urea then you can skip the NaOH as this is exactly what was told in my first post.

Please be more specific or let it go.
regards
ORG

so near, so far......

ApprenticeCook
(Hive Bee)
08-17-04 00:00
No 525811
      boom!

now thats bucket chem if i ever did see it...

You need to be sure of whats in it totally to see what you will get out and possible side rxns which may occur, as org said, you may just end up as wallpaper on the crumbled remains of your house via your method.

Any ammonium salt can be used with a base to produce ammonia gas.
Just be certain of the salts % contents if your using fert to see what may/will happen.

-AC

Its just my opinion, but no-one listens to me anyway, and rightly so...

armageddon
08-17-04 20:38
      ANFO
(Rated as: misinforming)

Organikum
(Wonderful Personality)
08-18-04 00:50
No 525975
      Huhu! Jemand zuhause? Ammonia anhydrous.

Huhu! Jemand zuhause?

Ammonia anhydrous. If you add LYE to ammonium nitrate you dont get anhydrous ammonia without extensive drying. If you add NaOH you will have problems in getting an mixture homogenous enough to prevent thermal decomposition - if this is possible at all.

Anhydrous, anhydrous, anhydrous - fuck did anybody read the subject of the thread?
Eh - yes, lets try again: Dis anybody UNDERSTAND the subject? And NaOH and lye are not interchangeable, arnt they?

Oh this hurts.

so near, so far......

armageddon
(Hive Bee)
08-18-04 01:41
No 525994
User Picture       my fault

My fault - I didn't think about it, just thought some water would be necessary to get them to react...
(of course drying is necessary when H2O is added)

If you add NaOH you will have problems in getting an mixture homogenous enough to prevent thermal decomposition - if this is possible at all

I don't think it is possible. Anyway, if Quantum meant mixing solid NaOH with solid fertilizer - I don't think it will react at any appreciable rate at all, even more unlikely that an explosion will occur. To get NH3(g) from solid fertilizer with the aid of NaOH, water has to be present...

And if the fertilizer consists of urea, simple heating should suffice of course, like you said... wink

Greetz A

Pleased to meet you hope you get my name.
But whats puzzlin you is the nature of my game!

ApprenticeCook
(Hive Addict)
08-18-04 05:05
No 526036
      q

Just to ask a question,
What is cyanuric acid useful for?

But the method is great, urea is dirt cheap and rather safe when compared to other methods of production, and if the urea is sufficiently dried then yes it would be an excellent way to get anhy ammonia for a dirt cheap basement door price!!! smile

-AC

Its just my opinion, but no-one listens to me anyway, and rightly so...

longimanus
(Hive Bee)
08-18-04 08:59
No 526060
      cyanuric acid

Preparation of trichloroisocyanuric acid from cyanuric acid:
Molecule: TCICUA ("OC1=NC(O)=NC(O)=N1.[K]OC2=NC(O[K])=NC(O[K])=N2.O=C(N(Cl)C(N3Cl)=O)N(Cl)C3=O")
Step 1: KOH
Step 2: Cl₂, UV, 0°C

And we all know what is trichloroisocyanuric acid used for.

psyloxy
(Hive Addict)
08-18-04 16:50
No 526089
User Picture       urea to TCCA...

urea to cyanuric acid
Patent US2822363
Patent US3093641
Patent US2872447
Patent US2527316
Patent US2790801
Patent US2943088
Patent US3297697
Patent US2952679
Patent US2975177
Patent DE865306
Patent DE752639

cyanuric acid to trichlorocyanuric acid
Patent US2969360
Patent DE1089764
Patent DE2226350

--psyloxy--

Lestat
(Hive Bee)
08-18-04 23:53
No 526140
User Picture       Trichloroisocyanuric acid is used in 99-100%...

Trichloroisocyanuric acid is used in 99-100% conc. as a swimming pool chemical I bee-lieve, I have seen it listed for sale at many pool shops online.

Kids, say NO to the DEA!

armageddon
(Hive Bee)
08-19-04 14:09
No 526298
User Picture       exactly

Yup, and it's very cheap - sold by the kilo...

Why bother with making it yourself? Doesn't seem worth the work!? (just curious about the intention behind it)

Greetz A

Pleased to meet you hope you get my name.
But whats puzzlin you is the nature of my game!

psyloxy
(Hive Addict)
08-19-04 15:17
No 526303
User Picture       doublethink

Uhm, well - you're completely right. Since the topic came up I wanted to throw in something useful. On second thought it seems futile to try and synth TCCA. OTOH maybe the urea to cyanuric acid patents are interesting in respect to the topic of this thread (I don't know).

--psyloxy--

armageddon
(Hive Bee)
08-20-04 16:34
No 526487
User Picture       no problem

In case you thought so: I didn't want to flame you - it was really pure interest...

Of course the patents about converting urea to cyanuric are quite interesting, seen in connection with this thread! wink

I just imagined on the one hand {all those solvents used, much work and cleaning up afterwards} vs. {walk-in and buy some kilos for some few bucks without any questions} OTOH smile .

Greetz A

Pleased to meet you hope you get my name.
But whats puzzlin you is the nature of my game!

ApprenticeCook
(Hive Addict)
08-22-04 01:41
No 526668
      ahem?

Why bother with making it yourself?
(in ref to tcca)Its not the main focus of what we want....

in org original post:
Urea + heat = cyanuric acid + ammonia
And the thread title:
NH3 - anhydrous
So the cyanuric acid is just another product of the heating to get out anhy ammonia.... were not interested in it at all... (in this thread anyway)
Infact the talk about cyanuric was started by foolish me when i asked what it was used for..... whoops! off topic!

So is there any further comment on org's method for anhy ammonia?
-AC

Its just my opinion, but no-one listens to me anyway, and rightly so...

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	All 17 posts		Subject: NH3 - anhydrous		Please login to post		Down


		Organikum (Wonderful Personality) 03-20-04 19:59 No 496351				NH3 - anhydrous (Rated as: good idea!)
						Sometimes the chemist would love to have some ammonia gas in its anhydrous form available in his laboratory without being forced to buy a gascylinder full of this compound which has gotten an somehow evil smell (it always was bad smelling of course) because of its inflationary use in the manufacture of methamphetamine from pseudoephedrine containing pills. How to produce this compound quick and easy and - anhydrous? The best method known to me by now was posted by lugh long time ago and used CaO and NH4Cl to free the ammonia from its salt. Drawback here is that water is formed in the reaction and an additional drying tower with CaO/NaOh is required for to get the ammonia almost anhydrous, another drawback is that CaO is not everywhere easily available, probably because of its properties in dissoving cadavers quick and complete. As I got interested in this ammonia lately - NO! Not for reductive amination purposes, but for use as fertilizer thats understood - I searched a lil´ bit and found this: 3CH4N2O + heat = C3H3N3O3 + 3NH3 Urea + heat = cyanuric acid + ammonia Preparation of cyanuric acid: ...More practically by heating urea until the evolution of ammonia ceases and the mass becomes solid again; .... REMARK: Urea melts at about 135°C. Cyanuric acid at about 330°C. I the reaction biuret is formed as an intermediate which melts/decomposes at about 190°C, so the favorable reaction temperature is between 200°C and 300°C. Even higher temperatures will even decompose the cyanuric acid to cyanic acid and CO2, whereby the cyanic acid will form NH3 with any water present, but its easier to stop at the cyanuric acid stage which is a valuable compound for its own in my eyes. Higher temperatures wont make any problems though. Ref: - Wöhlers Outline of Organic Chemistry, 1873, page 216ff. - MERCK Index 2002. Calculated yields (approx.): 410ml (~280gram) anhydrous ammonia (liquid@-34°C) from 1kg dry urea. Not sooo bad I want to say, for urea is dirtcheap, everywhere available and the procedure is not what I would call rocketscience. The procedure was tested and works. Shareholder of Paranoid Fucks inc.



		thermalpressure (Stranger) 08-09-04 18:24 No 524449				Generator setup uses
						May I ask what type of setup is to be used. Is a drying tower still necessary. What about a precooler would a regular spiral condenser suffice as a precooler.



		Organikum (Wonderful Personality) 08-09-04 18:43 No 524451				As told this produces ammonia without water...
						As told this produces ammonia without water (dry/dried urea is understood - dry it just below the docomposition temperature... ). As told the ammonia will be pretty hot though free from water. A iron or SS tube-spiral through icewater will suffice as precooler - a standard spriral glasscooler fed with icewater will suffice if the amount of ammonia is not to large. No copper, no brass but plain old iron/mild steel is perfectly ok here. Your question is not to answer universally as cooling depends on the amounts processed, heat transfer capability, temperature difference...and, and, and... hope this helps nevertheless. so near, so far......



		quantum (Hive Bee) 08-16-04 03:19 No 525632				try this
						put high ammonia containing fert with sodium hydroxide then heat too easy and fucking cheap e3500 console login: root bash-2.05#



		Organikum (Wonderful Personality) 08-16-04 05:56 No 525691				Hmmmmm....Re: put high ammonia containing fert
						Hmmmmm.... put high ammonia containing fert with sodium hydroxide then heat too easy and fucking cheap I dont know what this fertilizer exactly contains. Heating ammonium nitrate left a rather big hole in Oklahoma City lately AFAIK. If the fertilizer is urea then you can skip the NaOH as this is exactly what was told in my first post. Please be more specific or let it go. regards ORG so near, so far......



		ApprenticeCook (Hive Bee) 08-17-04 00:00 No 525811				boom!
						now thats bucket chem if i ever did see it... You need to be sure of whats in it totally to see what you will get out and possible side rxns which may occur, as org said, you may just end up as wallpaper on the crumbled remains of your house via your method. Any ammonium salt can be used with a base to produce ammonia gas. Just be certain of the salts % contents if your using fert to see what may/will happen. -AC Its just my opinion, but no-one listens to me anyway, and rightly so...



		armageddon 08-17-04 20:38				ANFO (Rated as: misinforming)



		Organikum (Wonderful Personality) 08-18-04 00:50 No 525975				Huhu! Jemand zuhause? Ammonia anhydrous.
						Huhu! Jemand zuhause? Ammonia anhydrous. If you add LYE to ammonium nitrate you dont get anhydrous ammonia without extensive drying. If you add NaOH you will have problems in getting an mixture homogenous enough to prevent thermal decomposition - if this is possible at all. Anhydrous, anhydrous, anhydrous - fuck did anybody read the subject of the thread? Eh - yes, lets try again: Dis anybody UNDERSTAND the subject? And NaOH and lye are not interchangeable, arnt they? Oh this hurts. so near, so far......



		armageddon (Hive Bee) 08-18-04 01:41 No 525994				my fault
						My fault - I didn't think about it, just thought some water would be necessary to get them to react... (of course drying is necessary when H2O is added) If you add NaOH you will have problems in getting an mixture homogenous enough to prevent thermal decomposition - if this is possible at all I don't think it is possible. Anyway, if Quantum meant mixing solid NaOH with solid fertilizer - I don't think it will react at any appreciable rate at all, even more unlikely that an explosion will occur. To get NH3(g) from solid fertilizer with the aid of NaOH, water has to be present... And if the fertilizer consists of urea, simple heating should suffice of course, like you said... Greetz A Pleased to meet you hope you get my name. But whats puzzlin you is the nature of my game!



		ApprenticeCook (Hive Addict) 08-18-04 05:05 No 526036				q
						Just to ask a question, What is cyanuric acid useful for? But the method is great, urea is dirt cheap and rather safe when compared to other methods of production, and if the urea is sufficiently dried then yes it would be an excellent way to get anhy ammonia for a dirt cheap basement door price!!! -AC Its just my opinion, but no-one listens to me anyway, and rightly so...



		longimanus (Hive Bee) 08-18-04 08:59 No 526060				cyanuric acid
						Preparation of trichloroisocyanuric acid from cyanuric acid: Molecule: TCICUA ("OC1=NC(O)=NC(O)=N1.[K]OC2=NC(O[K])=NC(O[K])=N2.O=C(N(Cl)C(N3Cl)=O)N(Cl)C3=O") Step 1: KOH Step 2: Cl₂, UV, 0°C And we all know what is trichloroisocyanuric acid used for.



		psyloxy (Hive Addict) 08-18-04 16:50 No 526089				urea to TCCA...
						urea to cyanuric acid Patent US2822363 Patent US3093641 Patent US2872447 Patent US2527316 Patent US2790801 Patent US2943088 Patent US3297697 Patent US2952679 Patent US2975177 Patent DE865306 Patent DE752639 cyanuric acid to trichlorocyanuric acid Patent US2969360 Patent DE1089764 Patent DE2226350 --psyloxy--



		Lestat (Hive Bee) 08-18-04 23:53 No 526140				Trichloroisocyanuric acid is used in 99-100%...
						Trichloroisocyanuric acid is used in 99-100% conc. as a swimming pool chemical I bee-lieve, I have seen it listed for sale at many pool shops online. Kids, say NO to the DEA!



		armageddon (Hive Bee) 08-19-04 14:09 No 526298				exactly
						Yup, and it's very cheap - sold by the kilo... Why bother with making it yourself? Doesn't seem worth the work!? (just curious about the intention behind it) Greetz A Pleased to meet you hope you get my name. But whats puzzlin you is the nature of my game!



		psyloxy (Hive Addict) 08-19-04 15:17 No 526303				doublethink
						Uhm, well - you're completely right. Since the topic came up I wanted to throw in something useful. On second thought it seems futile to try and synth TCCA. OTOH maybe the urea to cyanuric acid patents are interesting in respect to the topic of this thread (I don't know). --psyloxy--



		armageddon (Hive Bee) 08-20-04 16:34 No 526487				no problem
						In case you thought so: I didn't want to flame you - it was really pure interest... Of course the patents about converting urea to cyanuric are quite interesting, seen in connection with this thread! I just imagined on the one hand {all those solvents used, much work and cleaning up afterwards} vs. {walk-in and buy some kilos for some few bucks without any questions} OTOH . Greetz A Pleased to meet you hope you get my name. But whats puzzlin you is the nature of my game!



		ApprenticeCook (Hive Addict) 08-22-04 01:41 No 526668				ahem?
						Why bother with making it yourself? (in ref to tcca)Its not the main focus of what we want.... in org original post: Urea + heat = cyanuric acid + ammonia And the thread title: NH3 - anhydrous So the cyanuric acid is just another product of the heating to get out anhy ammonia.... were not interested in it at all... (in this thread anyway) Infact the talk about cyanuric was started by foolish me when i asked what it was used for..... whoops! off topic! So is there any further comment on org's method for anhy ammonia? -AC Its just my opinion, but no-one listens to me anyway, and rightly so...

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