Calcium hydroxyapatite based sulfonate grease compositions and method of manufacture

Patent metadata

Field	Value
Publication number	US-9458406-B2
Application number	US-201213664768-A
Country	US
Kind code	B2
Filing date	Oct 31, 2012
Priority date	Oct 31, 2011
Publication date	Oct 4, 2016
Grant date	Oct 4, 2016

Abstract

An overbased calcium sulfonate grease composition comprising a reduced amount of overbased calcium sulfonate, calcium hydroxyapatite, base oil, one or more converting agents, and one or more complexing acids if a complex grease is desired. The calcium sulfonate grease composition improves thickener yield and expected high temperature utility as demonstrated by dropping point. A method of making the composition comprising the steps of mixing the calcium sulfonate and base oil, adding the calcium carbonate either before or after conversion, adding one or more converting agents, and adding one or more complexing acids. All or a portion of one or more of the complexing acids may be added with or prior to the one or more converting agents.

First claim

I claim:

1. A calcium sulfonate grease composition comprising the following ingredients: overbased oil-soluble calcium sulfonate and calcium hydroxyapatite having a formula of Ca 5 (PO 4 ) 3 OH or mathematically equivalent formula with a melting point of around 1100 C.

2. The calcium sulfonate grease composition according to claim 1 comprising around 10% to 36% overbased oil-soluble calcium sulfonate.

3. The calcium sulfonate grease composition according to claim 2 wherein the grease has a worked 60 stroke penetration between 265 and 295 and a dropping point of 575 F or higher.

4. The calcium sulfonate grease composition according to claim 1 wherein the grease is a complex grease and comprises between 25% and 32% overbased oil-soluble calcium sulfonate.

5. The calcium sulfonate grease composition according to claim 1 further comprising the following ingredients: at least one converting agent and at least one complexing acid.

6. The calcium sulfonate grease composition according to claim 5 wherein the amount of calcium hydroxyapatite is stoichiometrically insufficient to neutralize all of the complexing acid.

7. The calcium sulfonate grease composition according to claim 6 further comprising one or more other basic calcium compounds selected from the group consisting of: calcium hydroxide, calcium oxide, added calcium carbonate or any combination thereof in a total amount sufficient to neutralize at least some of the complexing acid not neutralized by the calcium hydroxyapatite.

8. The calcium sulfonate grease composition according to claim 7 wherein the overbased oil-soluble calcium sulfonate comprises finely dispersed calcium carbonate and 5%-30% of that calcium carbonate is used to neutralize substantially all of the complexing acid not neutralized by the calcium hydroxyapatite and the one or more other basic calcium compounds.

9. The calcium sulfonate grease composition according to claim 5 wherein the amount of calcium hydroxyapatite is stoichiometrically sufficient to neutralize all of the complexing acid or acids.

10. The calcium sulfonate grease composition according to claim 9 further comprising one or more other basic calcium compounds selected from the group consisting of: calcium hydroxide, calcium oxide, added calcium carbonate or any combination thereof.

11. The calcium sulfonate grease composition according to claim 5 further comprising a facilitating acid.

12. The calcium sulfonate complex grease composition according to claim 9 wherein no calcium oxide or calcium hydroxide is added.

13. The calcium sulfonate complex grease composition according to claim 5 wherein the one or more converting agents are selected from the group consisting of alcohols, ethers, glycols, glycol ethers, glycol polyethers, carboxylic acids, inorganic acids, organic nitrates, compounds that contain active hydrogen or compounds that contain tautomeric hydrogen; and
wherein the one or more complexing acids are selected from the group consisting of a long chain carboxylic acid, a short chain carboxylic acid, boric acid, and phosphoric acid.

14. The calcium sulfonate complex grease composition according to claim 11 wherein the facilitating acid is dodecylbenzene sulfonic acid.

15. The calcium sulfonate grease composition according to claim 3 wherein the overbased calcium sulfonate is a poor quality overbased calcium sulfonate.

16. The calcium sulfonate grease composition according to claim 7 wherein the grease has a worked 60 stroke penetration between 265 and 295 and a dropping point of 575 F or higher.

17. The calcium sulfonate grease composition according to claim 16 wherein the overbased oil-soluble calcium sulfonate is a poor quality calcium sulfonate.

18. The calcium sulfonate grease composition according to claim 6 further comprising one or more basic calcium compounds selected from the group consisting of calcium oxide, calcium hydroxide, or a combination thereof, wherein the one or more other basic calcium compounds comprise equivalent basicity of no more than 75% of the hydroxide equivalent basicity provided by the total of the calcium hydroxyapatite and the one or more basic calcium compounds.

19. The calcium sulfonate grease composition according to claim 5 further comprising one or more basic calcium compounds selected from the group consisting of calcium oxide, calcium hydroxide, or a combination thereof, wherein the calcium hydroxyapatite and one or more basic calcium compounds are stoichiometrically insufficient to neutralize all of the complexing acid.

20. The calcium sulfonate grease composition according to claim 19 wherein the overbased oil-soluble calcium sulfonate comprises finely dispersed calcium carbonate and 5%-30% of that calcium carbonate is used to neutralize substantially all of the complexing acid not neutralized by the calcium hydroxyapatite and one or more basic calcium compounds.

21. A calcium sulfonate grease composition comprising the following ingredients:
around 10% to 36% overbased oil-soluble calcium sulfonate;
2% to 20% calcium hydroxyapatite having a formula of Ca 5 (PO 4 ) 3 OH or mathematically equivalent formula, excluding mixtures of true crystalline tricalcium phosphate and true crystalline calcium hydroxide by such equivalent formula;
2% to 10% water;
one or more other converting agents in a total amount of 0.1% to 5% and
one or more complexing acids in a total amount of 2.8% to 11%.

22. The calcium sulfonate grease composition according to claim 21 wherein the grease has a dropping point of 575 F or higher.

23. The calcium sulfonate grease composition according to claim 21 further comprising one or more other basic calcium compounds and wherein the amount of calcium hydroxyapatite is stoichiometrically insufficient to neutralize all of the complexing acid.

24. The calcium sulfonate grease composition according to claim 23 wherein the one or more other basic calcium compounds is selected from the group consisting of: calcium hydroxide, calcium oxide, added calcium carbonate or any combination thereof and wherein the total amount of the one or more other basic calcium compounds is at least stoichiometrically sufficient to neutralize all of the complexing acid not neutralized by the calcium hydroxyapatite.

25. The calcium sulfonate grease composition according to claim 24 wherein the overbased calcium sulfonate is a poor quality overbased calcium sulfonate.

26. The calcium sulfonate grease composition according to claim 21 further comprising one or more other basic calcium compounds selected from the group consisting of calcium oxide, calcium hydroxide, or a combination thereof, wherein the one or more other basic calcium compounds comprise equivalent basicity of no more than 75% of the hydroxide equivalent basicity provided by the total of the calcium hydroxyapatite and the one or more basic calcium compounds.

27. A method for making an overbased calcium sulfonate complex grease comprising the steps of:
mixing overbased oil-soluble calcium sulfonate having amorphous calcium carbonate dispersed therein with a base oil, and one or more converting agents to form a pre-conversion mixture;
converting the pre-conversion mixture to a converted mixture by heating until conversion of the amorphous calcium carbonate to crystalline calcium carbonate has occurred;
mixing calcium hydroxyapatite with the pre-conversion mixture or the convert

Assignees

• Waynick J Andrew
• Nch Corp

Inventors

• Waynick J Andrew

Classifications

• C10N2070/00

  Specific manufacturing methods for lubricant compositions · CPC title

• C10N2030/08

  Resistance to extreme temperature · CPC title

• C10N2050/10

  semi-solid; greasy · CPC title

• C10M2201/0856

  used as thickening agent · CPC title

• C10M135/10 Primary

  Sulfonic acids or derivatives thereof · CPC title