IP Library Granted Patent US 11,312,789
Granted Patent B2
US 11,312,789 · App. 15/533,381 · Granted Apr 26, 2022

Size reduction of ethylcellulose polymer particles

Inventors: Jorg Theuerkauf (Lake Jackson, TX); Robert B. Appell (Midland, MI); Peter E. Pierini (Lake Jackson, TX); Christopher J. Tucker (Midland, MI)
Assignee: NUTRITION & BIOSCIENCES USA 1, LLC
C08B11/20C08B11/08C08J3/05C08J3/12C08J2301/28F28D1/04
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Quick Facts
Patent No.
US 11,312,789
App. No.
15/533,381
Granted
Apr 26, 2022
Kind
B2
Abstract

Provided is a process for reducing the size of ethylcellulose polymer particles comprising (a) providing a slurry comprising (i) water (ii) said ethylcellulose particles, wherein said ethylcellulose polymer particles have D50 of 100 μm or less; (iii) surfactant comprising 1.2% or more anionic surfactants by weight based on the solid weight of said slurry, with the proviso that if the amount of anionic surfactant is 2.5% or less by weight based on the solid weight of said slurry, then said surfactant further comprises 5% or more stabilizers by weight based on the solid weight of said slurry, wherein said stabilizer is selected from the group consisting of water-soluble polymers, water-soluble fatty alcohols, and mixtures thereof. (b) grinding said slurry in an agitated media mill having a collection of media particles having a median particle size of 550 μm or smaller. Also provided is a dispersion made by such a process.

Claims (27)

1. A process for reducing the size of ethylcellulose polymer particles comprising

(a) providing a slurry comprising

(i) a continuous liquid medium comprising water

(ii) said ethylcellulose polymer particles, wherein said ethylcellulose polymer particles have D50 of 100 μm or less;

(iii) surfactant comprising 1.2% or more anionic surfactants by weight based on the solid weight of said slurry, with the proviso that if the amount of anionic surfactant is 2.5% or less by weight based on the solid weight of said slurry, then said surfactant further comprises 5% or more stabilizers by weight based on the solid weight of said slurry, wherein said stabilizer is selected from the group consisting of water-soluble polymers, water-soluble fatty alcohols, and mixtures thereof,

(b) grinding said slurry in an agitated media mill having a collection of grinding media particles having a median particle size of 550 μm or smaller,

wherein said grinding step comprises passing said slurry through said media mill to produce an intermediate slurry that exits said media mill via an exit; and then circulating said intermediate slurry through a loop comprising a heat exchanger and said media mill.

2. The process of claim 1 , wherein said intermediate slurry at said exit of said media mill is kept at a temperature of 9 to 15° C.

3. The process of claim 1 , wherein said surfactant comprises 2.5% or less anionic surfactants by weight based on the solid weight of said slurry, and wherein said surfactant additionally comprises 5% or more polyvinyl alcohol by weight based on the solid weight of said slurry.

4. The process of claim 1 , wherein said surfactant comprises 2.5% or less anionic surfactants by weight based on the solid weight of said slurry, and wherein said surfactant additionally comprises 5% or more water-soluble fatty alcohol by weight based on the solid weight of said slurry.

5. The process of claim 4 , wherein the water-soluble fatty alcohol molecule does not contain any sulfate, sulfonate, phosphate, or carboxylate groups.

6. The process of claim 4 , wherein the water-soluble fatty alcohol is a fatty ester having the structure of an ester of a fatty carboxylic acid with a multihydroxyl alcohol, in which one or more of the hydroxyl groups on the multihydroxyl alcohol remains as a hydroxyl group.

7. The process of claim 1 , wherein said ethylcellulose polymer has ethyl ether content of from 44% to 51%.

8. The process of claim 1 , wherein said surfactant comprises 2.5% or less anionic surfactants by weight based on the solid weight of said slurry, and wherein said surfactant additionally comprises 5% or more water-soluble polymer by weight based on the solid weight of said slurry, and wherein the water-soluble polymer is selected from the group consisting of polyvinyl alcohol, poly(N-vinyl pyrrolidone), and neutral water-soluble polymers that are derivatives of cellulose.

9. The process of claim 1 , wherein said ethylcellulose polymer has viscosity of from 2 mPa-s to 120 mPa-s.

10. The process of claim 1 , wherein said anionic surfactant has a single fatty group.

11. The process of claim 1 , wherein said anionic surfactant is selected from the group consisting of sulfates, sulfonates, phosphates, and carboxylates.

12. The process of claim 1 , wherein said anionic surfactant is a sulfate.

13. The process of claim 1 , wherein the amount of material other than water, ethylcellulose polymer, anionic surfactant, and stabilizer (if present) in the slurry is from 0 to 3% by weight based on the solid weight of the slurry.

14. The process of claim 1 , wherein said intermediate slurry at said exit of said media mill is kept at a temperature of 0 to 15° C.

15. The process of claim 1 further comprising generating an aqueous dispersion of ethylcellulose polymer particles having D90 of 2 μm or less.

16. The process of claim 1 , wherein the agitated media mill comprises one or more agitator that applies mechanical agitation to the grinding media particles.

17. The process of claim 16 , wherein the agitator comprises a rotating shaft with disks or pins or both attached therewith.

18. The process of claim 1 , wherein the continuous liquid medium comprises 80% or more of water by weight based on the weight of the continuous liquid medium.

19. The process of claim 1 , wherein the continuous liquid medium comprises 90% or more of water by weight based on the weight of the continuous liquid medium.

20. The process of claim 1 , wherein the temperature of said slurry is between 0° C. to 20° C.

21. The process of claim 1 , wherein the temperature of said slurry is from 6° C. to 15° C.

Assignments (4)
CHANGE OF LEGAL ENTITY Recorded Nov 28, 2020
From: DDP SPECIALTY ELECTRONIC MATERIALS US, INC.
To: DDP SPECIALTY ELECTRONIC MATERIALS US, LLC.
Reel/Frame 054530/0384 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 28, 2020
From: DOW GLOBAL TECHNOLOGIES LLC
To: THE DOW CHEMICAL COMPANY
Reel/Frame 054531/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 28, 2020
From: THE DOW CHEMICAL COMPANY
To: DDP SPECIALTY ELECTRONIC MATERIALS US, INC.
Reel/Frame 054533/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 28, 2020
From: DDP SPECIALTY ELECTRONIC MATERIALS US, LLC.
To: NUTRITION & BIOSCIENCES USA 1, LLC
Reel/Frame 054533/0575 →