Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid

Patent metadata

Field	Value
Publication number	US-10087388-B2
Application number	US-201715593839-A
Country	US
Kind code	B2
Filing date	May 12, 2017
Priority date	May 18, 2016
Publication date	Oct 2, 2018
Grant date	Oct 2, 2018

Abstract

A method of making an overbased calcium sulfonate or calcium magnesium sulfonate grease using one or more delay periods between the addition of at least a portion of a facilitating acid, such as DDBSA, and at least a portion of the next subsequently added ingredient. The delay period may be a temperature adjustment delay or a holding delay period. An overbased calcium sulfonate or calcium magnesium sulfonate grease composition comprises 0.5%-5% of a facilitating acid, allows for a reduced amount of overbased calcium sulfonate below 22%, and allows for a reduced amount of calcium hydroxyapatite to provide 10-25% of hydroxide equivalent basicity of the total hydroxide equivalent basicity due to calcium hydroxyapatite and added calcium hydroxide, while maintaining a high dropping point.

First claim

We claim:

1. A method of making an overbased calcium sulfonate grease or an overbased calcium-magnesium sulfonate grease comprising:
adding and mixing an amount of overbased calcium sulfonate containing amorphous calcium carbonate dispersed therein, an optional base oil, and an amount of facilitating acid to form an initial mixture;
adding and mixing one or more converting agents to the initial mixture 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;
optionally adding and mixing an amount of overbased magnesium sulfonate with the initial mixture, pre-conversion mixture, the converted mixture, or a combination thereof; and
wherein there is one or more facilitating acid delay periods between the addition of the facilitating acid and at least a portion of any subsequently added ingredient; and
wherein the one or more facilitating acid delay periods comprise:
a facilitating acid holding delay period where the initial mixture is held at a temperature or range of temperatures for a period of time of 20 minutes or more between adding the facilitating acid and the subsequent addition of at least a portion of another ingredient, or
a facilitating acid temperature adjustment delay period where the initial mixture is heated or cooled to a temperature or range of temperatures after adding the facilitating acid and prior to the subsequent addition of at least a portion of another ingredient, or
a combination thereof.

2. The method of claim 1 wherein the amount of overbased calcium sulfonate is 10-45% and the amount of optional overbased magnesium sulfonate is 0.1-30%.

3. The method of claim 1 wherein the amount of overbased calcium sulfonate is 10-36% and the amount of optional overbased magnesium sulfonate is 1-24%.

4. The method of claim 1 wherein the amount of overbased calcium sulfonate is 10-30% and the amount of optional overbased magnesium sulfonate is 1-20%.

5. The method of claim 1 wherein the amount of overbased calcium sulfonate is 10-22% and the amount of optional overbased magnesium sulfonate is 1-15%.

6. The method of claim 1 wherein there is at least one facilitating acid temperature adjustment delay period where the initial mixture is heated to a temperature range of 190-200 F after adding the facilitating acid and prior to the subsequent addition of at least a portion of another ingredient.

7. The method of claim 6 wherein there is at least one facilitating acid holding delay period where the initial mixture is held at a temperature range of 190-200 F for around 20-30 minutes prior to the subsequent addition of at least a portion of another ingredient.

8. The method of claim 7 wherein the subsequently added ingredient added after the facilitating acid holding delay period is magnesium sulfonate, calcium hydroxyapatite, or calcium carbonate.

9. The method of claim 1 further comprising adding and mixing one or more calcium containing bases with the initial mixture, the pre-conversion mixture, the converted mixture, or a combination thereof;
adding and mixing one or more complexing acids with the pre-conversion mixture, the converted mixture, or both;
wherein water is one of the converting agents;
wherein there is one or more magnesium sulfonate delay periods between the addition of any one of water, one of the calcium containing bases, one of the complexing acids, the facilitating acid, or any portion thereof and the addition of at least a portion of the overbased magnesium sulfonate; and
wherein one of the facilitating acid delay periods may be simultaneous with one of the magnesium sulfonate delay periods;
wherein the one or more magnesium sulfonate delay periods comprise:
a magnesium sulfonate holding delay period where the mixture comprising water, one of the calcium containing bases, one of the complexing acids, the facilitating acid, or any portion thereof is maintained at a temperature or within a range of temperatures for a period of time prior to adding at least a portion of the magnesium sulfonate, or
a magnesium sulfonate temperature adjustment delay period wherein the mixture comprising water, one of the calcium containing bases, one of the complexing acids, the facilitating acid, or any portion thereof is heated or cooled prior to adding at least a portion of the magnesium sulfonate; or
a combination thereof.

10. The method of claim 1 wherein water is one of the converting agents and wherein the water is added after at least one facilitating acid delay period.

11. The method of claim 1 wherein water is one of the converting agents and wherein water is not present during any facilitating acid delay period.

12. The method of claim 1 wherein a first portion of the magnesium sulfonate is added to the pre-conversion mixture and a second portion of the magnesium sulfonate is added to the converted mixture.

13. The method of claim 12 wherein around 10-50% of the total amount of magnesium sulfonate is added as the first portion.

14. The method of claim 12 further comprising adding and mixing one or more calcium containing bases with the pre-conversion mixture, the converted mixture, or both;
adding and mixing one or more complexing acids with the pre-conversion mixture, the converted mixture, or both; and
wherein water is one of the converting agents.

15. The method of claim 14 wherein the calcium containing bases are calcium hydroxyapatite, added calcium carbonate, added calcium hydroxide, added calcium oxide or a combination thereof.

16. The method of claim 15 wherein the calcium containing bases comprise calcium hydroxyapatite and calcium hydroxide and wherein the calcium hydroxyapatite contributes around 10% or more of the hydroxide equivalent basicity of the total hydroxide equivalent basicity due to calcium hydroxyapatite and added calcium hydroxide.

17. The method of claim 16 wherein the calcium hydroxyapatite contributes around 10% to 25% of the hydroxide equivalent basicity of the total hydroxide equivalent basicity due to calcium hydroxyapatite and added calcium hydroxide.

18. The method of claim 14 wherein one of the converting agents is a non-aqueous converting agent and wherein there is one or more converting agent delay periods between the addition of water and the addition of at least a portion of the non-aqueous converting agent;
wherein the one or more converting agent delay periods comprise:
a converting agent holding delay period where the mixture comprising water as a converting agent is maintained at a temperature or within a range of temperatures for a period of time prior to adding at least a portion of the non-aqueous converting agent, or
a converting agent temperature adjustment delay period wherein the mixture comprising water as a converting agent is heated or cooled prior to adding at least a portion of the non-aqueous converting agent, or
a combination thereof.

19. The method of claim 18 wherein the amount of water added as a converting agent is 1.5-10% and the total amount of non-aqueous converting agents is 0.1-5%.

20. The method of claim 18 wherein the ratio of overbased calcium sulfonate to overbased magnesium sulfonate in the pre-conversion mixture is in a range from about 20:1 to 100:1.

21. The method of claim 1 further comprising adding and mixing an alkali metal hydroxide with the pre-conversion mixture, the converted mixture, or both.

22

Assignees

• Nch Corp

Inventors

• Waynick J Andrew
• Garza Jr Joe L

Classifications

• C10M121/04 Primary

  Reaction products · CPC title

• C10N2050/10

  semi-solid; greasy · CPC title

• C10N2010/04

  Groups 2 or 12 · CPC title

• C10N2070/00

  Specific manufacturing methods for lubricant compositions · CPC title

• C10N2030/08

  Resistance to extreme temperature · CPC title