# US 10,122,052 B2 · Systems and methods for purifying and recycling lead from spent lead-acid batteries

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- Number: US 10,122,052 B2
- Document ID: US10122052B2
- Status: Granted
- Kind: B2
- Application number: 15/674,028
- Filed: 2017-08-10
- Published: 2017-11-23
- Granted: 2018-11-06
- Earliest claimed: 2014-06-20
- Assignees: Johnson Controls Technology Company
- Applicants: Johnson Controls Technology Company
- Inventors: Matthew A. Spence; Patrick M. Curran
- Web page: https://patentgrep.com/patent/US10122052B2

## CPC

- H01M 10/54: Reclaiming serviceable parts of waste accumulators
- B01J 6/001: {Calcining}
- B01J 6/002: {using rotating drums}
- B01J 8/008: {Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction (B01J8/0285, B01J8/067, B01J8/087, B01J8/1836 take precedence)}
- B01J 19/06: Solidifying liquids (making microcapsules B01J13/02)
- B01J 19/2465: {externally, i.e. the mixture leaving the vessel and subsequently re-entering it}
- C22B 3/02: Apparatus therefor
- C22B 3/04: by leaching (C22B3/18 takes precedence)
- C22B 7/006: {Wet processes}
- C22B 7/007: {by acid leaching}
- C22B 7/009: {General processes for recovering metals or metallic compounds from spent catalysts (for recovering specific metals C22B11/00 - C22B61/00)}
- C22B 13/04: {by wet processes}
- C22B 13/045: {Recovery from waste materials}
- H01M 6/52: Reclaiming serviceable parts of waste cells or batteries {, e.g. recycling}
- B01J 2208/00805: Details of the particulate material
- Y02P 10/20: Recycling
- Y02W 30/84: Recycling of batteries or fuel cells
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT

## Abstract

The present disclosure relates to systems and methods by which lead from spent lead-acid batteries may be extracted, purified, and used in the production of new lead-acid batteries. The system includes a first phase separation device configured to: receive the first mixture from the basic lead stream digestion device, isolate a liquid component from one or more insoluble components of the first mixture, and output the liquid component. The system also includes a lead salt precipitation device configured to: receive and mix the liquid component and a carboxylate source to form a second mixture including a lead salt precipitate, and output the second mixture. The system further includes a second phase separation device configured to: receive the second mixture from the lead salt precipitation device, isolate the liquid component from the lead salt precipitate of the second mixture, and output the lead salt precipitate.

## Claims

### Claim 1

A system, comprising:
a basic lead stream digestion device configured to: receive and mix a hydroxide and a lead-bearing material to form a first mixture, and output the first mixture;
a first phase separation device configured to: receive the first mixture from the basic lead stream digestion device, isolate a liquid component from one or more insoluble components of the first mixture, and output the liquid component;
a lead salt precipitation device configured to: receive and mix the liquid component and a carboxylate source to form a second mixture comprising a lead salt precipitate, and output the second mixture;
a second phase separation device configured to: receive the second mixture from the lead salt precipitation device, isolate the liquid component from the lead salt precipitate of the second mixture, and output the lead salt precipitate; and
a rotary kiln calciner configured to: receive the lead salt precipitate from the second phase separation device, introduce the lead salt precipitate into a top of a rotating tube furnace of the rotary kiln calciner, mix the lead salt precipitate with a gaseous stream to oxidize the lead salt precipitate into leady oxide within the rotating tube furnace, and output the leady oxide at a bottom of the rotating tube furnace.

### Claim 2 (depends on 1)

The system of claim 1, comprising a lead-acid battery processing device configured to: receive at least one lead-acid battery, grind the at least one lead-acid battery into the lead-bearing material, and to output the lead-bearing material.

### Claim 3 (depends on 1)

The system of claim 1, comprising a impurity gas removal device configured to: receive the liquid component from the first phase separation device, mix the liquid component with a compound that evolves one or more impurity gases from one or more impurities of the liquid component, and output the liquid component to the lead salt precipitation device without the one or more impurities.

### Claim 4 (depends on 1)

The system of claim 1, wherein the pH of the first mixture in the basic lead stream digestion device is greater than 7.

### Claim 5 (depends on 1)

The system of claim 1, wherein the pH of the first mixture in the basic lead stream digestion device is between 8 and 14.

### Claim 6 (depends on 1)

The system of claim 1, wherein the first phase separation device comprises a filter press, a clarifier, or a cyclone separator.

### Claim 7 (depends on 1)

The system of claim 1, wherein the second phase separation device comprises a belt dryer or a spray dryer configured to: remove the lead salt precipitate from the second mixture, and heat and dry the lead salt precipitate.

### Claim 8 (depends on 7)

The system of claim 7, wherein the belt dryer is further configured to at least partially oxidize the lead salt precipitate into leady oxide while heating and drying the lead salt precipitate.

### Claim 9 (depends on 1)

The system of claim 1, wherein the pH of the second mixture in the lead salt precipitation device is 7 or below.

### Claim 10 (depends on 1)

The system of claim 1, wherein the pH of the second mixture in the lead salt precipitation device is between approximately 2 and approximately 6.

### Claim 11 (depends on 1)

The system of claim 1, wherein the leady oxide comprises between approximately 0% and approximately 35% free lead.

### Claim 12 (depends on 1)

The system of claim 1, wherein the leady oxide comprises leady oxide particles having a D50 between approximately 0.2 μm and approximately 20 μm.

### Claim 13 (depends on 1)

The system of claim 1, wherein the leady oxide has a BET surface area greater than approximately 2.5 square meters per gram (m2/g).

### Claim 14 (depends on 1)

The system of claim 1, wherein the leady oxide has an acid absorption greater than approximately 250 milligrams H2SO4 per gram.

### Claim 15 (depends on 1)

The system of claim 1, wherein the leady oxide comprises less than approximately 20% beta phase lead oxide.

### Claim 16

A system, comprising:
a basic lead stream digestion device configured to: receive and mix a hydroxide and a lead-bearing material to form a first mixture, and output the first mixture;
a first phase separation device configured to: receive the first mixture from the basic lead stream digestion device, isolate a liquid component from one or more insoluble components of the first mixture, and output the liquid component;
a lead salt precipitation device configured to: receive and mix the liquid component and a carboxylate source to form a second mixture comprising a lead salt precipitate, and output the second mixture;
a second phase separation device configured to: receive the second mixture from the lead salt precipitation device, isolate the liquid component from the lead salt precipitate of the second mixture, and output the lead salt precipitate; and
a spray calciner configured to: receive the lead salt precipitate from the second phase separation device, atomize the lead salt precipitate, mix the atomized lead salt precipitate with a gaseous stream to oxidize the lead salt precipitate into leady oxide particles, and output the leady oxide particles.

### Claim 17

A system, comprising:
a basic lead stream digestion device configured to: receive and mix a hydroxide and a lead-bearing material to form a first mixture, and output the first mixture;
a first phase separation device configured to: receive the first mixture from the basic lead stream digestion device, isolate a liquid component from one or more insoluble components of the first mixture, and output the liquid component;
a lead salt precipitation device configured to: receive and mix the liquid component and a carboxylate source to form a second mixture comprising a lead salt precipitate, and output the second mixture;
a second phase separation device configured to: receive the second mixture from the lead salt precipitation device, isolate the liquid component from the lead salt precipitate of the second mixture, and output the lead salt precipitate; and a stirred pot reactor configured to: receive the lead salt precipitate from the second phase separation device, mix the lead salt precipitate with a gaseous stream using an agitator to oxidize the lead salt precipitate into leady oxide, and output the leady oxide.
