IP Library Granted Patent US 11,407,842
Granted Patent B2
US 11,407,842 · App. 16/608,892 · Granted Aug 9, 2022

Method for controlled preparation of low molecular weight cellulose ether

Inventors: Robert B. Appell (Wilmington, DE); Joseph L Weir (Wilmington, DE)
Assignee: NUTRITION & BIOSCIENCES USA 1, LLC
C08B11/08
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Quick Facts
Patent No.
US 11,407,842
App. No.
16/608,892
Granted
Aug 9, 2022
Kind
B2
Abstract

A process includes: (a) providing an initial cellulose ether powder containing 0.5 to 10 weight-percent water based on total cellulose ether powder weight; (b) heating the initial cellulose ether powder to a temperature in a range of 30 to 130 degrees Celsius; (c) before, during and/or after heating in step (b), adding solid base to the cellulose ether powder and mixing with the initial cellulose ether powder to form a cellulose ether/base mixture; (d) adding volatile acid to the cellulose ether/base mixture and mixing; and (e) allowing the volatile acid to hydrolyze the initial cellulose ether to form a final cellulose ether having a lower viscosity than the initial cellulose ether.

Claims (19)

1. A process comprising:

(a) providing an initial cellulose ether powder comprising 0.5 to 10 weight-percent water based on total cellulose ether powder weight;

(b) heating the initial cellulose ether powder to a temperature in a range of 30 to 130 degrees Celsius;

(c) before, during and/or after heating in step (b), adding a solid base to the initial cellulose ether powder and mixing the solid base with the initial cellulose ether powder to form a uniform mixture of the solid base and the initial cellulose ether powder;

(d) adding a volatile acid to the cellulose ether/base mixture and mixing; and

(e) allowing the volatile acid to hydrolyze the initial cellulose ether to form a final cellulose ether having a lower viscosity than the initial cellulose ether,

wherein the solid base is selected from the group consisting of bicarbonate salts, carbonate salts, basic alumina, weak base resins, strong base resins, and mixtures thereof.

2. The process of claim 1 , wherein the amount of the volatile acid added in step (d) is 0.08 to 0.5 weight-percent based on initial cellulose ether powder weight and the molar amount of the solid base added in step (c) is 0.4 to 1.25 times the number of moles of the volatile acid added in step (d).

3. The process of claim 1 , wherein an additional base is added after adding the volatile acid in step (d).

4. The process of claim 1 , wherein the initial cellulose ether powder is selected from the group consisting of methyl cellulose, hydroxypropyl methylcellulose, and mixtures thereof.

5. The process of claim 1 , wherein the solid base is dry sodium bicarbonate powder.

6. The process of claim 5 , wherein the volatile acid is anhydrous hydrogen chloride.

7. The process of claim 1 , wherein the initial cellulose ether powder has viscosity of more than 2,000 millipascal*seconds.

8. The process of claim 1 , wherein the final cellulose ether has a viscosity in a range of one to 25,000 millipascal*seconds.

9. The process of claim 8 , wherein the final cellulose ether has a viscosity in a range of one to 4,000 millipascal*seconds.

10. The process of claim 1 , wherein the final cellulose ether has a pH in a range of 5-8.

11. The process of claim 1 , wherein the final cellulose ether comprises less than 20 weight-parts formaldehyde per million weight-parts final cellulose ether without a step of removing formaldehyde from the final cellulose ether.

12. The process of claim 1 , wherein the volatile acid is selected from the group consisting of hydrogen halide, formic acid, and combinations thereof.

13. The process of claim 12 , wherein the volatile acid is anhydrous hydrogen chloride.

Assignments (5)
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 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 28, 2019
From: APPELL, ROBERT B; WEIR, JOSEPH L.
To: DOW GLOBAL TECHNOLOGIES LLC
Reel/Frame 050837/0803 →
Continuity (2)
Provisional Application 62546046 · Aug 16, 2017
Related Publication 20200181290A1 · Jun 11, 2020