| Pages:
1
..
8
9
10 |
Hey Buddy
Hazard to Others
Posts: 429
Registered: 3-11-2020
Location: Bushwhacker Country
Member Is Offline
|
|
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]
|
|
|
Axt
National Hazard
Posts: 795
Registered: 28-1-2003
Member Is Offline
Mood: No Mood
|
|
I you are desperate enough, you could extract the nickel hydroxide from dead NiMh batteries.
|
|
|
pdb
Hazard to Self
Posts: 80
Registered: 8-4-2004
Member Is Offline
Mood: No Mood
|
|
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
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1387
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
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)
|
|
|
Etanol
Hazard to Others
Posts: 188
Registered: 27-2-2012
Member Is Offline
Mood: No Mood
|
|
| 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
|
Bad idea. Ni(AGu)2(ClO4)2 and Ni(AGu)2(NO3)2 mix formed.
|
|
|
| Pages:
1
..
8
9
10 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
