Microencapsulation of chemical additives

Patent metadata

Field	Value
Publication number	US-10611983-B2
Application number	US-201515311119-A
Country	US
Kind code	B2
Filing date	May 15, 2015
Priority date	May 15, 2014
Publication date	Apr 7, 2020
Grant date	Apr 7, 2020

Abstract

The present disclosure relates to new and optimized processes for the preparation of micro- and nano-scale capsules containing lubricant chemical additives. The present disclosure also relates to micro- and nano-scale capsules prepared by such processes, which are useful in a variety of applications, including automotive lubricants, diesel lubricants, industrial lubricants, metal-working lubricants, coolants, and process fluids. Micro-and nano-scale capsules prepared as described herein have the required properties that such capsules need to exhibit in order to function effectively and meet the requirements imposed by engine lubrication conditions. The microcapsules may be dispersed in a lubricating oil such that the lubricant exhibits improved stability and anti-wear performance, thereby improving engine fuel efficiency and performance.

First claim

What is claimed is:

1. A process for preparing microcapsules of a lubricant additive, the process comprising
(i) forming an aqueous solution comprising one or more emulsifiers;
(ii) adding one or more curing catalyst and one or more cross-linking agent to the product of step (i) at a pH of between about 2 and about 5 to form an emulsion under stirring at about 500 to about 1000 rpm;
(iii) adding a first lubricant additive to the emulsion of step (ii);
(iv) adding a solution comprising (i) formaldehyde, paraformaldehyde or a combination thereof, and (ii) urea, melamine, or a combination thereof, to the product of step (iii); and
(v) heating the product of step (iv) to form microcapsules of the lubricant additive, wherein
(a) the microcapsules have a size between about 2 microns and about 40 microns, and
(b) the shell or membrane enclosing the microcapsule core is (i) stable at a temperature of at least 200° C., and (ii) is of sufficient mechanical strength to be stable at a shear level of at least 1 GPa.

2. The process of claim 1 , wherein the curing catalyst is selected from ammonium chloride and the cross-linking agent is selected from resorcinol.

3. The process of claim 1 , wherein the molar ratio of (i) formaldehyde, paraformaldehyde or a combination thereof, to (ii) urea, melamine, or a combination thereof, is about 1 to about 3.

4. The process according to claim 1 , further comprising
(vi) cooling the resulting microcapsules; and
(vii) isolating the microcapsules.

5. The process according to claim 4 , wherein step (vii) further comprises washing the microcapsules with one or more solvents.

6. The process according to claim 1 , wherein the emulsifier is selected from the group consisting of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, dioctyl sulfosuccinate sodium, poly(ethylene-alt-maleic anhydride), gum arabic, hexadecyltrimethylammonium bromide, poly(vinyl alcohol), poly(styrene-co-maleic anhydride), polyethylene glycol, polypropylene glycol, polyoxyethylene octyl phenyl ether, polysorbates, sorbitan esters, and any combination thereof.

7. The process according to claim 1 , wherein the lubricant additive is selected from the group consisting of antioxidants, detergents, dispersants, antiwear additives, surface deactivators, acid neutralizing agents, lubricant film enhancers, smart viscosity modifiers, corrosion inhibitors, rust inhibitors, high base materials, reparative agents, power point depressants, seal compatibility agents, antifoam agents, viscosity index improvers, heat transfer agents, surface reactivity control agents, and any combination thereof.

8. The process according to claim 1 , wherein the microcapsules have a size between about 2 and about 30 microns.

9. The process according to claim 1 , wherein the microcapsules have a cell thickness of between about 0.4 and about 2 microns.

10. A microcapsule comprising one or more lubricant additives, prepared by a process according to claim 1 .

11. The process according to claim 1 , wherein the emulsifier is selected from the group consisting of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, dioctyl sulfosuccinate sodium, poly(ethylene-alt-maleic anhydride), hexadecyltrimethylammonium bromide, poly(vinyl alcohol), poly(styrene-co-maleic anhydride), polyethylene glycol, polypropylene glycol, polyoxyethylene octyl phenyl ether, polysorbates, sorbitan esters, and any combination thereof.

12. The process of claim 1 , wherein the molar ratio of (i) formaldehyde, paraformaldehyde or a combination thereof, to (ii) urea, melamine, or a combination thereof, is about 1.5 to about 2.5.

13. The process of claim 1 , wherein the molar ratio of (i) formaldehyde, paraformaldehyde or a combination thereof, to (ii) urea, melamine, or a combination thereof, is about 1 to about 1.9.

14. The process according to claim 1 , wherein the microcapsules have a size between about 3 and about 28 microns.

15. The process according to claim 1 , wherein the microcapsules have a cell thickness of between about 0.4 and about 0.5 microns.

16. A process for preparing microcapsules of a lubricant additive, the process comprising
(i) forming an aqueous solution consisting essentially of one or more emulsifiers selected from the group consisting of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, dioctyl sulfosuccinate sodium, poly(ethylene-alt-maleic anhydride), hexadecyltrimethylammonium bromide, poly(vinyl alcohol), poly(styrene-co-maleic anhydride), polyethylene glycol, polypropylene glycol, polyoxyethylene octyl phenyl ether, polysorbates, sorbitan esters, and any combination thereof;
(ii) adding one or more curing catalyst and one or more cross-linking agent to the product of step (i) at a pH of between about 2 and about 5 to form an emulsion under stirring at about 500 to about 1000 rpm;
(iii) adding a first lubricant additive to the emulsion of step (ii);
(iv) adding a solution comprising (i) formaldehyde, paraformaldehyde or a combination thereof, and (ii) urea, melamine, or a combination thereof, to the product of step (iii); and
(v) heating the product of step (iv) to form microcapsules of the lubricant additive, wherein
(a) the microcapsules have a size between about 2 microns and about 40 microns, and
(b) the shell or membrane enclosing the microcapsule core is (i) stable at a temperature of at least 200° C., and (ii) is of sufficient mechanical strength to be stable at a shear level of at least 1 GPa.

17. The method of claim 1 , wherein the microcapsules of the lubricant additive exhibits enhanced thermal stability and/or anti-wear performance compared to the lubricant additive not in the form of microcapsules.

18. The method of claim 1 , wherein the microcapsules of the lubricant additive are stable under contact pressures up to about 800 MPa.

19. The method of claim 1 , wherein step (iv) comprises adding a solution comprising formaldehyde and urea to the product of step (iii).

20. The method of claim 1 , wherein step (iv) comprises adding a solution comprising formaldehyde and melamine to the product of step (iii).

21. The method of claim 1 , wherein step (iii) comprises adding two or more lubricant additives.

22. The method of claim 16 , wherein step (iii) comprises adding two or more lubricant additives.

Assignees

• Univ George Washington

Inventors

• Hsu Stephen M
• Zhao Fei

Classifications

• C10N2050/12

  Micro capsules · CPC title

• C10N2030/10

  Inhibition of oxidation, e.g. anti-oxidants · CPC title

• B01J13/14 Primary

  Polymerisation; cross-linking · CPC title

• C11D17/0039

  Coated compositions or coated components in the compositions, (micro)capsules · CPC title

• C10N2030/06

  Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure · CPC title