Process for preparing transition metal hydroxides

Patent metadata

Field	Value
Publication number	US-9630842-B2
Application number	US-201213344784-A
Country	US
Kind code	B2
Filing date	Jan 6, 2012
Priority date	Jan 10, 2011
Publication date	Apr 25, 2017
Grant date	Apr 25, 2017

Abstract

The present invention relates to a process for preparing transition metal hydroxides with a mean particle diameter in the range from 6 to 12 μm (D50), which comprises combining, in a stirred vessel, at least one solution of at least one transition metal salt with at least one solution of at least one alkali metal hydroxide to prepare an aqueous suspension of transition metal hydroxide, and, in at least one further compartment, continuously introducing a mechanical power in the range from 50 to 10 000 W/l in a proportion of the suspension in each case, based on the proportion of the suspension, and then recycling the proportion into the stirred vessel.

First claim

The invention claimed is:

1. A process for preparing transition metal hydroxides having a mean particle diameter in the range from 6 to 12 μm (D50), the process comprising:
combining, in a stirred vessel, a solution of a transition metal salt with a solution of an alkali metal hydroxide to prepare an aqueous suspension of transition metal hydroxide;
continuously withdrawing a volume of the suspension from the stirred vessel and supplying to at least one separately powered compartment;
continuously introducing, in the at least one separately powered compartment, a mechanical power in the range from 50 to 10,000 W/l in each case, based on the volume of the suspension; and then
recycling the volume from said at least one separately powered compartment back into the stirred vessel.

2. The process according to claim 1 , wherein the transition metal is at least one selected from the group consisting of Cr, V, Mn, Ni, Fe, Co, Zn, and mixtures of one or more of the aforementioned with one another or with alkali metal, aluminum or magnesium.

3. The process according to claim 1 wherein an overall mean power in the range from 2 to 25 W/l is introduced based on overall suspension.

4. The process according to claim 1 , wherein at least 20% of the mechanical power introduced overall is introduced at a power density of from 50 to 10,000 W/l.

5. The process according to claim 1 , wherein the separately powered compartment is at least one selected from the group consisting of a pump, an insert, a mixing unit, a wet mill, a stirred tank and a homogenizer.

6. The process according to claim 1 , wherein the separately powered compartment is connected to the stirred vessel via a pumped circulation system.

7. The process according to claim 1 , wherein a mean solids content of the suspension in the range from 70 to 1000 g/l is employed.

8. The process according to claim 1 , wherein the transition metal is selected from mixtures of Ni, Mn, Co and optionally at least one further metal selected from the group consisting of alkali metal, aluminum and magnesium.

9. The process according to claim 1 , wherein precipitated transition metal hydroxide is removed from a mother liquor, and particles with a diameter greater than 50 μm are removed.

10. The process according claim 9 , wherein particles of transition metal hydroxide with a diameter greater than 30 μm are removed.

Assignees

• Krippels Uwe
• Schroedle Simon
• Basf Se

Inventors

• Krippels Uwe
• Schroedle Simon

Classifications

• 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

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C01B13/363

  Mixtures of oxides or hydroxides by precipitation · CPC title

• H01M4/505

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

• C01G53/44

  containing manganese · CPC title