IP Library Granted Patent US 11,613,685
Granted Patent B2
US 11,613,685 · App. 16/554,498 · Granted Mar 28, 2023

Oil-in-water macro-emulsion process for forming solid gel beads meltable to form a gel phase change material

Inventors: Madison B. Hammerberg (Union, OH); Jessica P. Davis (Kettering, OH)
Assignee: Microtek Laboratories, Inc.
C09K5/06C08F212/08
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Quick Facts
Patent No.
US 11,613,685
App. No.
16/554,498
Granted
Mar 28, 2023
Kind
B2
Abstract

Solid gel beads formed from a gel product of a 5 carbon to 60 carbon alkane phase change material, 5 carbon to 60 carbon alkene phase change material, or a combination thereof and a styrene-based polymer are homogeneous, has an uneven exterior surface, and a major axis length in a range of 1000 μm to 100 mm. Methods for making the solid gel bead include providing water having a preselected temperature based on a linear relationship to the melting point of a phase change material composition, mixing the phase change material composition with the styrene-based polymer at or below the preselected temperature with stirring to form a pulp, and mixing the pulp into the water with turbulent mixing while maintaining the temperature of the mixture at the preselected temperature.

Claims (33)

1. A method for making solid gel bead, the method comprising:

providing water having a preselected temperature based on a linear relationship to the melting point of a phase change material composition expressed as Y=0.6X+45 (±1° C. up to ±7° C.), wherein X is the melting point of the phase change material in degrees Celsius and Y is the preselected temperature in degrees Celsius;

mixing the phase change material composition comprising a 5 carbon to 60 carbon alkane phase change material, 5 carbon to 60 carbon alkene phase change material, or combinations thereof with a styrene-based polymer at or below the preselected temperature with stirring to form a pulp;

mixing the pulp into the water with turbulent mixing while maintaining the temperature of the mixture at the preselected temperature, thereby forming solid, homogenous gel beads without forming a viscoelastic liquid at any point within the process;

separating the solid, homogeneous gel beads from any remaining liquid.

2. The method of claim 1 , wherein the styrene-based polymer is a styrene-ethylene-butylene-styrene triblock copolymer.

3. The method of claim 2 , wherein an emulsion is created under pressure.

4. The method of claim 1 , wherein mixing to form the pulp is performed at standard temperature and pressure.

5. The method of claim 1 , wherein the turbulent mixing is maintained for a period of at least 5 minutes.

6. The method of claim 1 , wherein the turbulent mixing is maintained for 5 minutes to 30 minutes.

7. A continuous manufacturing method for making solid gel beads, the method comprising:

providing a source of water having a preselected temperature based on a linear relationship to the melting point of a phase change material composition expressed as Y=0.6X+45 (±1° C. up to ±7° C.), wherein X is the melting point of the phase change material in degrees Celsius and Y is the preselected temperature in degrees Celsius;

providing a vessel of a pulp mixture of a phase change material composition comprising a 5 carbon to 60 carbon alkane and/or a 5 carbon to 60 carbon alkene phase change material and a styrene-based polymer at or below the preselected temperature of the water;

introducing the pulp and the water into a turbulent mixer, thereby forming solid, homogenous gel beads without forming a viscoelastic liquid at any point within the process;

separating the solid gel beads from any remaining liquid;

drying the solid gel beads; and

distributing an allotment of dry solid gel beads into a container.

8. The method of claim 7 , wherein separating comprises a continuous screen or belt filter downstream of the turbulent mixer.

9. The method of claim 7 , wherein the turbulent mixer is a static mixer.

10. The method of claim 7 , wherein providing a source of water comprises heating the water prior to introducing the water into the turbulent mixer.

11. The method of claim 7 , wherein the pulp in the vessel is maintained at a temperature of 25° C. to 140° C. with mixing.

12. The method of claim 7 , wherein the pulp is mixed and maintained at standard temperature and pressure.

13. The method of claim 7 , wherein the styrene-based polymer is a styrene-ethylene-butylene-styrene triblock copolymer.

14. The method of claim 7 , wherein the method has yield greater than 90%.

15. The method of claim 7 , wherein the container is an end use container, and the method further comprises:

heating the end use container to melt the solid gel beads, thereby forming a liquid gel that conforms to the shape of the end use container; and

subsequently, cooling the end use container to form a solid gel in the shape of the end use container.

16. The method of claim 7 , wherein the container is a mold, and the method further comprises:

heating the mold to melt the solid gel beads, thereby forming a viscoelastic liquid that conforms to the shape of the mold; and

subsequently, cooling the mold to form a solid gel in the shape of the end use container.

17. The method of claim 7 , wherein the container is a shipping container.

18. The method of claim 7 , wherein the container is a plastic bag or pouch sealingly closed to retain the solid gel beads therein.

19. The method of claim 7 , wherein the container is a vessel for heating the solid gel beads and extruding therefrom a viscoelastic liquid resulting from heating the solid gel beads above the glass transition temperature thereof.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 30, 2026
From: MICROTEK HOLDINGS, INC.
To: ALEXIUM INTERNATIONAL GROUP LIMITED
Reel/Frame 073646/0553 →
CHANGE OF NAME Recorded May 29, 2025
From: MICROTEK LABORATORIES, INC.
To: MICROTEK HOLDINGS, INC.
Reel/Frame 071460/0399 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 10, 2019
From: HAMMERBERG, MADISON B.; DAVIS, JESSICA P.
To: MICROTEK LABORATORIES, INC.
Reel/Frame 050677/0586 →
Continuity (2)
Provisional Application 62724124 · Aug 29, 2018
Related Publication 20200071586A1 · Mar 5, 2020