Process for coating an oxide material

Patent metadata

Field	Value
Publication number	US-11515525-B2
Application number	US-201816489895-A
Country	US
Kind code	B2
Filing date	Feb 21, 2018
Priority date	Mar 8, 2017
Publication date	Nov 29, 2022
Grant date	Nov 29, 2022

Abstract

The present invention is related to a process for coating anoxide material, said process comprising the following steps: (a) providing a particulate material selected from lithiated nickel-cobalt aluminum oxides, lithiated cobalt-manganese oxides and lithiated layered nickel-cobalt-manganese oxides, (b) treating said cathode active material with a metal alkoxide or metal amide or alkyl metal compound, (c) treating the material obtained in step (b) with moisture, and, optionally, repeating the sequence of steps (b) and (c), wherein steps (b) and (c) are carried out in a mixer that mechanically introduces mixing energy into the particulate material, or by way of a moving bed or fixed bed, and wherein steps (b) and (c) are carried out at a pressure that is in the range of from 5 mbar to 1 bar above normal pressure.

First claim

The invention claimed is:

1. A process for coating an oxide material, comprising:
(a) providing a particulate material chosen from lithiated nickel-cobalt aluminum oxides according to formula Li[Ni h Co i Al j ]O 2+r , lithiated cobalt-manganese oxides according to formula Li 1+x (Co e Mn f M 4 d ) 1−x O 2 and lithiated layered nickel-cobalt-manganese oxides according to formula Li (1+x) [Ni a Co b Mn c M 4 d ] (1−x) O 2 ,
(b) treating the particulate material with a metal alkoxide, metal amide, or alkyl metal compound,
(c) treating the material obtained in (b) with moisture, and, optionally, repeating the sequence of (b) and (c),
wherein (b) and (c) are carried out in a vessel or cascade of at least tow vessels using a mixer that mechanically introduces mixing energy into the particulate material, or by way of a moving bed, or fixed bed, and
wherein (b) and (c) are carried out at a pressure ranging from 5 mbar to 1 bar above 1 atm,
wherein:
M 4 is chosen from Mg, Ca, Ba, Al, Ti, Zr, Zn, Mo, V and Fe,
zero≤x≤0.2,
0.1≤a≤0.8,
zero≤b≤0.5,
0.1≤c≤0.6,
zero≤d≤0.1, and a+b+c+d=1,
e is in a range of from 0.2 to 0.8,
f is in a range of from 0.2 to 0.8, and e+f+d=1,
h is in a range of from 0.8 to 0.90,
i is in a range of from 0.15 to 0.19,
j is in a range of from 0.01 to 0.05, and
r is in a range of from zero to 0.4; and
wherein particles of lithiated nickel-cobalt aluminum oxide or lithiated layered nickel-cobalt-manganese oxide, respectively, are cohesive having a Geldart C grouping: and
wherein particles of lithiated nickel-cobalt aluminum oxide or lithiated layered nickel-cobalt-manganese oxide, respectively, are cohesive having a flowability factor ff c ≤7.

2. The process according to claim 1 , wherein the mixer that mechanically introduces mixing energy into the particulate material is a compulsory mixer or a free-fall mixer.

3. The process according to claim 1 , wherein the alkyl metal compound, metal alkoxide, or metal amide has a formula chosen from M 1 (R 1 ) 2 , M 2 (R 1 ) 3 , M 3 (R 1 ) 4−y H y , M 1 (OR 2 ) 2 , M 2 (OR 2 ) 3 , M 3 (OR 2 ) 4 , M 3 [NR 2 ) 2 ] 4 , and methyl alumoxane wherein:
R 1 are each independently chosen from straight-chain C 1 -C 8 -alkyl and branched C 1 -C 8 -alkyl,
R 2 are each independently chosen from straight-chain C 1 -C 4 -alkyl and branched C 1 -C 8 -alkyl,
M 1 is Mg or Zn,
M 2 is Al or B,
M 3 is chosen from Si, Sn, Ti, Zr, and Hf, and
the variable y ranges from zero to 4.

4. The process according to claim 1 , wherein (b) is performed at 10 mbar to 150 mbar above 1 bar.

5. The process according to claim 1 , wherein (b) and (c) are performed in a rotating vessel that has baffles.

6. The process according to claim 1 , further comprising treating exhaust gases with water at a pressure above 1 atm.

7. The process according to claim 6 , wherein the exhaust gases are treated with water at a pressure ranging from 5 mbar to 1 bar above 1 atm.

8. The process according to claim 1 , wherein (b) is performed at a temperature in a range of from 15° C. to 350° C.

9. The process according to claim 1 , further comprising flushing a reactor with an inert gas between (b) and (c).

10. The process according to claim 1 , further comprising removing the coated oxide material from the vessel or vessels, respectively, by pneumatic convection.

11. The process according to claim 1 , wherein the particulate material has an average particle diameter (D 50 ) ranging from 3 μm to 20 μm.

12. The process according to claim 1 , wherein the particulate material has a BET surface area ranging from 0.1 m 2 /g to 1 m 2 /g.

13. The process according to claim 1 , wherein the amount of metal alkoxide or metal amide or alkyl metal compound ranges from 0.1 g to 1 g per 1 kg of the particulate material.

14. The process according to claim 1 , wherein progress of the process is controlled by mass spectrometry.

Assignees

• Basf Se

Inventors

• Kleine Jaeger Frank
• Liebsch Tillmann
• Schoenherr Michael
• Garella Dominik
• Cetinel Fatih
• Sommer Heino
• Ahlf Maraike
• Loeffler Daniel
• Vogelsang Regina
• Haag Jacob

Classifications

• C23C16/442

  using fluidised bed process · CPC title

• C23C16/40

  Oxides · CPC title

• H01M4/525

  of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy · CPC title

• H01M4/505

  of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy · CPC title

• H01M4/62

  Selection of inactive substances as ingredients for active masses, e.g. binders, fillers · CPC title