Oxidized carbon blacks and applications for lead acid batteries

Patent metadata

Field	Value
Publication number	US-9923205-B2
Application number	US-201615211406-A
Country	US
Kind code	B2
Filing date	Jul 15, 2016
Priority date	Jul 17, 2015
Publication date	Mar 20, 2018
Grant date	Mar 20, 2018

Abstract

Disclosed herein are oxidized carbon blacks, which can be incorporated into electrode compositions for lead acid batteries. In some embodiments, the oxidized carbon blacks have a BET surface area ranging from 650 to 2100 m 2 /g; an oil absorption number (OAN) ranging from 35 to 500 mL/100 g; and a volatile content of at least 5.5 wt. % relative to the total weight of the oxidized carbon black, as determined by weight loss at 950° C.

First claim

The invention claimed is:

1. An oxidized carbon black having the following properties:
a BET surface area ranging from 650 to 2100 m 2 /g;
an oil absorption number (OAN) ranging from 35 to 500 mL/100 g; and
at least one of the following properties:
(a) a volatile content of at least 5.5 wt. % relative to the total weight of the oxidized carbon black, as determined by weight loss at 950° C.;
(b) a total oxygen content of at least 3.5 wt. % relative to the total weight of the oxidized carbon black;
(c) a total titratable acidic group content of at least 0.5 μmol/m 2 , as determined by Boehm's titration method; and
(d) a total titratable acidic group content of at least 0.5 mmol/g, as determined by Boehm's titration method.

2. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has a BET surface area ranging from 650 to 1500 m 2 /g.

3. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has an OAN ranging from 35 to 200 mL/100 g.

4. The oxidized carbon black of claim 1 , wherein the oxidized carbon black is derived from the base carbon black, in which the base carbon black has a primary particle size ranging from 8 to 50 nm.

5. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has a conductivity index ranging from 10 to 75, where the conductivity index is derived from the following equation:
Conductivity Index=[BET×OAN]1/2/[1+volatile content].

6. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has a powder resistivity of at least 0.2 Ω-cm.

7. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has a pH ranging from 1.5 to 6, as determined by ASTM D1512.

8. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has a concentration of surface carboxylic groups ranging from 0.15 mmol/g to 1.5 mmol/g, or from 0.1 μmol/m 2 to 1.2 μmol/m 2 , as determined by Boehm's titration method.

9. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has a surface energy ranging from 25 mJ/m 2 to 50 mJ/m 2 .

10. The oxidized carbon black of claim 1 , wherein the oxidized carbon black has a crystallite size (La) ranging from 16 Å to 23 Å, as determined by Raman spectroscopy.

11. An electrode comprising:
an oxidized carbon black having a BET surface area ranging from 80 to 2100 m 2 /g, wherein the oxidized carbon black has at least one of the following properties:
(a) a volatile content of at least 3 wt. % relative to the total weight of the oxidized carbon black, as determined by weight loss at 950° C.;
(b) a total oxygen content of at least 3.5 wt. % relative to the total weight of the oxidized carbon black;
(c) a total titratable acidic group content of at least 0.5 μmol/m 2 , as determined by Boehm's titration method; and
(d) a total titratable acidic group content of at least 0.5 mmol/g, as determined by Boehm's titration method.

12. The electrode of claim 11 , wherein the oxidized carbon black has an oil absorption number (OAN) ranging from 35 to 360 mL/100 g.

13. The electrode of claim 11 , wherein the oxidized carbon black has a concentration of surface carboxylic groups ranging from 0.15 mmol/g to 1.5 mmol/g, or from 0.1 μmol/m 2 to 1.2 μmol/m 2 , as determined by Boehm's titration method.

14. The electrode of claim 11 , wherein the oxidized carbon black has a pH ranging from 1.5 to 6, as determined by ASTM D1512.

15. The electrode of claim 11 , wherein the oxidized carbon black has a surface energy ranging from 25 mJ/m 2 to 50 mJ/m 2 .

16. The electrode of claim 11 , wherein the oxidized carbon black has a crystallite size (La) ranging from 16 Å to 23 Å, as determined by Raman spectroscopy.

17. A lead acid battery comprising the electrode of claim 11 .

18. A method of making an oxidized carbon black, comprising:
oxidizing a base carbon black, in which the base carbon black has a BET surface area ranging from 650 to 2100 m 2 /g and an oil absorption number (OAN) ranging from 35 to 500 mL/100 g;
wherein the oxidized carbon black has at least one of the following properties:
(a) a volatile content of at least 5.5 wt. % relative to the total weight of the oxidized carbon black, as determined by weight loss at 950° C.;
(b) a total oxygen content of at least 3.5 wt. % relative to the total weight of the oxidized carbon black;
(c) a total titratable acidic group content of at least 0.5 μmol/m 2 , as determined by Boehm's titration method; and
(d) a total titratable acidic group content of at least 0.5 mmol/g, as determined by Boehm's titration method.

19. The method of claim 18 , wherein the oxidized carbon black has a concentration of surface carboxylic groups ranging from 0.15 mmol/g to 1.5 mmol/g, or from 0.1 μmol/m 2 to 1.2 μmol/m 2 , as determined by Boehm's titration method.

20. The method of claim 18 , wherein the oxidized carbon black has a surface energy ranging from 25 mJ/m 2 to 50 mJ/m 2 , or a crystallite size (La) ranging from 16 Å to 23 Å, as determined by Raman spectroscopy.

Assignees

• Cabot Corp

Inventors

• Korchev Andriy
• Dupasquier Aurelien
• Atanassova Paolina

Classifications

• H01M4/56

  of lead · CPC title

• H01M4/625 Primary

  Carbon or graphite · CPC title

• C01P2006/12

  Surface area · CPC title

• H01M4/14

  Electrodes for lead-acid accumulators · CPC title

• C09C1/565 Primary

  comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone · CPC title