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Hey Buddy
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Quote: Originally posted by pdb  |
Does anyone know how to properly prepare NiCO3 from Ni nitrate? Otherwise, I just need to double the amount of my suspect nickel carbonate in the
synthesis.
[Edited on 20-11-24 by pdb] |
I know a guy who prepares it through NiCl2 metathesis which worked well, and changes color between the two Ni salts for visual confirmation.
Just for reference, NiCO3 is available widely as a glaze component from any ceramic supply shop across the world. In the US, it is around $18-25/lb.
[Edited on 20-11-2024 by Hey Buddy]
[Edited on 20-11-2024 by Hey Buddy]
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Axt
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I you are desperate enough, you could extract the nickel hydroxide from dead NiMh batteries.
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pdb
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This time, I followed example 2.3 from the patent and Microtek's advice:
Synthesis of Hexaammine Nickel(II) Perchlorate Ni(NH3)6(ClO4)2
Ni(NO3)2·6H2O + 6 NH3 (aq) → Ni(NH3)6(NO3)2 + 6 H2O
Ni(NH3)6(NO3)2 + 2 HClO4 → Ni(NH3)6(ClO4)2 + 2 HNO3
- 2 g of Ni(NO3)2·6H2O in 5 ml of H2O
- add 1.86 g of NH3 (aq)
- add 1.57 g of 70% HClO4
Instead of attempting to isolate Ni(NH3)6(ClO4)2, the synthesis continues according to the patent:
- add 55 ml of H2O
- add 4.08 g of 70% HClO4
- add 3.81 g of aminoguanidine hydrogen carbonate
- after effervescence, fast heating until boiling, kept for 5 mn: the solution turns gray.
- ultrasonicating 4x5 mn: no precipitation occurs until the temperature drops to around 30°C.
The filtrate continues to deposit some NAP over the following hours.
However, the yield is only 32%, far from the 89% claimed in the patent
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Laboratory of Liptakov
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water solution: Ni(NO3)2 - anhydride 10g + NaHCO3 9,2g = 6,5g NiCO3 (insoluble) + 9,3g NaNO3 (hi soluble) + 2,4g CO2 + 0,1 H2O
water solution: NiCl2 (anhydride brown) 10g + 13g NaHCO3 = 14g Ni(HCO3)2 (insoluble in water) + NaCl
water solution: NiSO4 (anhydride) 10g + 10.9 NaHCO3 = 7.7g NiCO3 (insoluble) + Na2SO4 9.2g + CO2 2.8g + H2O 1.1g
Procedure from Ni(NO3)2: 2g Ni(NO3)2 hexahydrate insert as crystalls into glass + 2g NaHCO3 as dry powder added. Add 40g dH2O and temperaure
increase on 80 C on waterbath. Partially open cap was used. After 60 min. at 80 C is solution decantated, added 100g normal water, washing and
decantated or separated on Buchner device. After drying you have fine and pure powder of NiCO3...
 
[Edited on 22-11-2024 by Laboratory of Liptakov]
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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Etanol
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| Quote: Originally posted by pdb |
Instead of attempting to isolate Ni(NH3)6(ClO4)2, the synthesis continues according to the patent:
- add 55 ml of H2O
- add 4.08 g of 70% HClO4
- add 3.81 g of aminoguanidine hydrogen carbonate
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Bad idea. Ni(AGu)2(ClO4)2 and Ni(AGu)2(NO3)2 mix formed.
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Microtek
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Yes, the advantage of isolating the Ni(NH3)6(ClO4)2 is the absence of any ions that might interfere with the reaction, ensuring that whatever you get
really must be NAP. Also, I would suggest heating the AQ*HClO4 solution close to boiling before adding the Ni(NH3)6(ClO4)2.
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pdb
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| Quote: Originally posted by Laboratory of Liptakov |
Procedure from Ni(NO3)2: 2g Ni(NO3)2 hexahydrate insert as crystalls into glass + 2g NaHCO3 as dry powder added. Add 40g dH2O and temperaure
increase on 80 C on waterbath. Partially open cap was used. After 60 min. at 80 C is solution decantated, added 100g normal water, washing and
decantated or separated on Buchner device. After drying you have fine and pure powder of NiCO3 |
Thank you LL. There is a typo I guess... you mean 4 g (or more precisely 3.46 g) of Ni(NO3)2.6H2O
Heating the solution like this allows the decomposition of NiCO3 hydrates or hydroxides?
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Laboratory of Liptakov
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In short, such proportions that the baking soda is in excess over the reacting nickel nitrate. For example, by 10% by weight. Because baking soda is
much cheaper than nitrate, which needs to be used as much as possible in the production of NiCO3.
Decompositions on hydrates and hydroxides was not examinated at heating....
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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pdb
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| Quote: Originally posted by Axt |
Solution 1
Displacing AG bicarbonate with hydrochloride
2CH7N4.HCO3 + 2HCl --> 2CH7N4.Cl + 2H2O + 2CO2
Freebasing aminoguanidine
2CH7N4.Cl + 2NaOH --> 2CH6N4 + 2NaCl + 2H2O
Solution 2
Dissolution of nickel perchlorate
NiO + 2HClO4 --> Ni(ClO4)2 + H2O
Combine 1 & 2
Complexing aminoguanidine to nickel perchlorate
Ni(ClO4)2 + 2CH6N4 --> Ni(CH6N4)2(ClO4)2
Replace the HCl with HClO4 if the chloride complex has too low of a solubility. I feel like nickel oxide is more readily available than the carbonate
or nickel metal itself. |
I attempted this protocol with strictly stoichiometric proportions. Solution 1 was brought to a boil under magnetic stirring. Upon adding solution 2,
the solution turned gray-brown immediatly, and a greenish deposit appeared—CH7N4.Cl or what? After 5 minutes of boiling, the beaker was placed in an
ultrasonic bath, which produced nothing until the temperature dropped to around 30°C. At that point, a brick-red precipitate appeared along with red
needles on the surface.
In all my experiments with uNAP, I noticed that ultrasonication was ineffective as long as the solution temperature had not dropped to around 30°C.
Can everyone confirm this?
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Hey Buddy
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| Quote: Originally posted by pdb | | Quote: Originally posted by Axt |
Solution 1
Displacing AG bicarbonate with hydrochloride
2CH7N4.HCO3 + 2HCl --> 2CH7N4.Cl + 2H2O + 2CO2
Freebasing aminoguanidine
2CH7N4.Cl + 2NaOH --> 2CH6N4 + 2NaCl + 2H2O
Solution 2
Dissolution of nickel perchlorate
NiO + 2HClO4 --> Ni(ClO4)2 + H2O
Combine 1 & 2
Complexing aminoguanidine to nickel perchlorate
Ni(ClO4)2 + 2CH6N4 --> Ni(CH6N4)2(ClO4)2
Replace the HCl with HClO4 if the chloride complex has too low of a solubility. I feel like nickel oxide is more readily available than the carbonate
or nickel metal itself. |
I attempted this protocol with strictly stoichiometric proportions. Solution 1 was brought to a boil under magnetic stirring. Upon adding solution 2,
the solution turned gray-brown immediatly, and a greenish deposit appeared—CH7N4.Cl or what? After 5 minutes of boiling, the beaker was placed in an
ultrasonic bath, which produced nothing until the temperature dropped to around 30°C. At that point, a brick-red precipitate appeared along with red
needles on the surface.
In all my experiments with uNAP, I noticed that ultrasonication was ineffective as long as the solution temperature had not dropped to around 30°C.
Can everyone confirm this?
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Yes, it is supposed to be 20 C. It also is disrupted if the temp is really low, like when an ice bath is used. The target temp is 20 C and there
shouldnt be any needle crystals. The appearance of needle crystals probably means the transmission of sonication is not effective. Needle crystals
should be unable to form.
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Axt
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I would think the initial "green/brown" would be something more akin to a basic nickel perchlorate precipitating (not knowing anything of the
properties of Ni(OH)ClO4). Did it redissolve?
How did you make the Nickel perchlorate solution? using NiO + HClO4? I've never done this, but it will go through a basic nickel perchlorate
intermediate if it works.
Are the successful ultrasonicated precipitates using the bare solution or immersing a beaker in the ultrasonic bath? That may be your issue.
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pjig
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Is this axt that helped developing water gels?
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Axt
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Offtopic Watergel http://www.sciencemadness.org/talk/viewthread.php?tid=3214
| Quote: Originally posted by pdb | | Quote: Originally posted by Axt |
Solution 1
Displacing AG bicarbonate with hydrochloride
2CH7N4.HCO3 + 2HCl --> 2CH7N4.Cl + 2H2O + 2CO2
Freebasing aminoguanidine
2CH7N4.Cl + 2NaOH --> 2CH6N4 + 2NaCl + 2H2O
Solution 2
Dissolution of nickel perchlorate
NiO + 2HClO4 --> Ni(ClO4)2 + H2O
Combine 1 & 2
Complexing aminoguanidine to nickel perchlorate
Ni(ClO4)2 + 2CH6N4 --> Ni(CH6N4)2(ClO4)2
Replace the HCl with HClO4 if the chloride complex has too low of a solubility. I feel like nickel oxide is more readily available than the carbonate
or nickel metal itself. |
I attempted this protocol with strictly stoichiometric proportions. Solution 1 was brought to a boil under magnetic stirring. Upon adding solution 2,
the solution turned gray-brown immediatly, and a greenish deposit appeared—CH7N4.Cl or what? After 5 minutes of boiling, the beaker was placed in an
ultrasonic bath, which produced nothing until the temperature dropped to around 30°C. At that point, a brick-red precipitate appeared along with red
needles on the surface.
In all my experiments with uNAP, I noticed that ultrasonication was ineffective as long as the solution temperature had not dropped to around 30°C.
Can everyone confirm this?
|
Ok, curiosity got the better of me this is what works and what doesn't.
The method as posted works, but the problem is you cannot use the stoichiometric quantity to dissolve the NiO, it's just too hard to get in solution
even when run hot and concentrated. I was left with a lot of NiO unreacted. Taking the prep to the end, pouring in the NaOH resulted in an immediate
dump of the brick red precipitate but heavily contaminated with oxide.
Here's the better way,
Use the total acids needed to dissolve the NiO, this provides the excess needed to get the NiO into solution.
1.5g (0.02mol) nickel oxide and 11.5g (0.08mol) 70% perchloric acid in 20ml water.
Heat with stirring on 150 degree hotplate (solution temp 75 rising to 90) until a slurry with no black oxide left. Dilute and redissolve with 50ml
water for a clear emerald green.
Add 5.44g (0.04mol) aminoguanidine bicarbonate in 50ml, this will neutralise with the excess acid, you've now a dirty green solution of Ni(ClO4)2 and
2CH6N4.HClO4 in 100ml water.
A slight excess 3.74g (0.05mol) 25% ammonia is added, it turns dark purplish blue.
If left stand Ni(CH6N4)2(ClO4)2 precipitates out as brick coloured needles. This takes maybe 10 minutes. Use NaOH instead and its instant and less
controllable. Mixing was all done at room temp.
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pdb
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This time, the precipitation of uNAP took only 5-6 minutes with ultrasound. After filtration, I observed something I’ve noticed before: if the
washing with water is prolonged too much, the precipitate develops a gray film within a few minutes. I suppose this is the decomposition by water
mentioned by others? I don't have any IPA on hand; I need to get some.
[Edited on 28-11-24 by pdb]
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Hey Buddy
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| Quote: Originally posted by pdb | This time, the precipitation of uNAP took only 5-6 minutes with ultrasound. After filtration, I observed something I’ve noticed before: if the
washing with water is prolonged too much, the precipitate develops a gray film within a few minutes. I suppose this is the decomposition by water
mentioned by others? I don't have any IPA on hand; I need to get some.
[Edited on 28-11-24 by pdb] |
Yes
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