# US 2015/0147643 A1 · Purified Metal Complex Having Oxalic Acid as Ligand, and Method For Producing Purified Solution of Said Metal Complex in Non-Aqueous Solvent

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- Number: US 2015/0147643 A1
- Document ID: US20150147643A1
- Status: Published application
- Kind: A1
- Application number: 14/404,271
- Filed: 2013-05-29
- Published: 2015-05-28
- Earliest claimed: 2012-05-30
- Assignees: Central Glass Company, Limited
- Applicants: Central Glass Co., Ltd.
- Inventors: Takayoshi Morinaka; Satoshi Muramoto; Yoshinori Tateishi; Keiji Sato
- Web page: https://patentgrep.com/patent/US20150147643A1

## CPC

- H01M 10/0568: characterised by the solutes
- C07B 63/02: by treatment giving rise to a chemical modification
- C07F 5/022: {without C-boron linkages}
- C07F 9/65742: {non-condensed with carbocyclic rings or heterocyclic rings or ring systems}
- C07F 9/65744: {condensed with carbocyclic or heterocyclic rings or ring systems}
- H01G 11/54: Electrolytes
- H01M 4/382: {Lithium (H01M4/405 takes precedence)}
- H01M 10/05: Accumulators with non-aqueous electrolyte (H01M10/39 takes precedence)
- H01M 10/052: Li-accumulators
- H01G 11/58: Liquid electrolytes
- H01M 2300/0025: Organic electrolyte
- Y02E 60/10: Energy storage using batteries
- Y02E 60/13: Energy storage using capacitors
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C07B: GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR (preparation of carboxylic acid esters by telomerisation C07C67/47; telomerisation C08F)
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- H01G: CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE (selection of specified materials as dielectric H01B3/00; capacitors having potential barriers H10D1/62, H10K10/10)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

The present invention provides a purified metal complex having oxalic acid as a ligand and a method for industrially producing a purified non-aqueous solvent solution of the metal complex at low cost. In the method of the present invention, oxalic acid contained in a non-aqueous solvent solution of a metal complex having oxalic acid as a ligand is decomposed by a reaction with a thionyl halide in a non-aqueous solvent, and the decomposition product of the reaction and the unreacted thionyl halide are removed by deaeration.

## Claims

### Claim 1

A method for producing a purified non-aqueous solvent solution of a metal complex having oxalic acid as a ligand, from a non-aqueous solvent solution of a metal complex having oxalic acid as a ligand and containing oxalic acid as an impurity by decomposing and removing oxalic acid contained as an impurity in the non-aqueous solvent solution of a metal complex having oxalic acid as a ligand and containing oxalic acid as an impurity,
wherein the oxalic acid contained in the solution as an impurity is decomposed by a reaction with a thionyl halide in a non-aqueous solvent; and a decomposition product of the reaction and an unreacted thionyl halide are removed by deaeration.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the thionyl halide is at least one selected from the group consisting of thionyl chloride and thionyl bromide.

### Claim 3 (depends on 1)

The method according to claim 1 wherein the metal complex having oxalic acid as a ligand is at least one selected from the group consisting of difluoro(oxalato)borate, bis(oxalato)borate, difluorobis(oxalato)phosphate, tetrafluoro(oxalato)phosphate, tris(oxalato)phosphate and a mixture thereof.

### Claim 4 (depends on 1)

The method according to claim 1, wherein the counter cation of the metal complex having oxalic acid as a ligand is at least one counter cation selected from the group consisting of a lithium ion, a sodium ion, a potassium ion and a tetraalkylammonium ion.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the reaction and decomposition with the thionyl halide is performed at a temperature in a range of 10° C. to 100° C.

### Claim 6 (depends on 1)

The method according to claim 1, wherein the reaction decomposition product and the unreacted portion of the thionyl halide are removed by deaeration at a temperature in a range of 0° C. to 150° C.

### Claim 7 (depends on 1)

The method according to any one of claim 1, wherein oxalic acid and a thionyl halide are reacted at a molar ratio in a range of 1:0.1 to 1:10.

### Claim 8 (depends on 1)

The method according to claim 1, wherein oxalic acid and a thionyl halide are reacted at a molar ratio in a range of 1:1 to 1:10.

### Claim 9 (depends on 1)

A method according to claim 1, further comprising purification by crystallization after the removal.

### Claim 10 (depends on 1)

A purified non-aqueous solvent solution of a metal complex having oxalic acid as a ligand prepared by the production method according to claim 1.

### Claim 11 (depends on 9)

A purified metal complex having oxalic acid as a ligand prepared by the production method according to claim 9.

### Claim 12 (depends on 1)

A non-aqueous electrolyte battery comprising at least a cathode, an anode made of lithium or an anode material capable of occluding and releasing lithium, and an electrolytic solution for a non-aqueous electrolyte battery composed of a non-aqueous solvent and a solute, wherein the non-aqueous electrolyte battery comprises the purified metal complex having oxalic acid as a ligand and/or the purified non-aqueous solvent solution of a metal complex having oxalic acid as a ligand, prepared by the production method according to claim 1.
