Process of preparing an ester of a cellulose ether

Patent metadata

Field	Value
Publication number	US-9453081-B2
Application number	US-201314384220-A
Country	US
Kind code	B2
Filing date	Mar 12, 2013
Priority date	Mar 27, 2012
Publication date	Sep 27, 2016
Grant date	Sep 27, 2016

Abstract

A reaction product mixture is obtained from a reaction of (a) a cellulose ether with (b) an aliphatic monocarboxylic acid anhydride or with a di- or tricarboxylic acid anhydride or with a combination of an aliphatic monocarboxylic acid anhydride and a di- or tricarboxylic acid anhydride in the presence of (c) an aliphatic carboxylic acid. A process for precipitating an esterified cellulose ether from this reaction product mixture comprises the step of contacting the reaction product mixture with water and subjecting the combination of water and the reaction product mixture to a shear rate of at least 800 s −1 . The precipitated esterified cellulose ether can be recovered as a non-tacky product.

First claim

The invention claimed is:

1. A process for precipitating hydroxypropyl methyl cellulose acetate succinate (HPMCAS) from a reaction product mixture obtained from a reaction of (a) a hydroxypropyl methyl cellulose with (b) acetic anhydride and succinic anhydride the presence of (c) an aliphatic carboxylic acid, wherein the process comprises the step of
contacting the reaction product mixture having a temperature of 60-110° C. with water and subjecting the combination of water and the reaction product mixture to a shear rate of at least 800 s −1 wherein the HPMCAS forms a finely dispersed precipitate,
separating the dispersed HPMCAS from the remainder of the combination of water and reaction product mixture,
washing the HPMCAS with water to obtain a granular, non-sticking HPMCAS and
drying the washed HPMCAS to produce HPMCAS in the form of a powder.

2. The process of claim 1 wherein the reaction product mixture has been obtained from a reaction of (a) the hydroxypropyl methyl cellulose with (b) acetic anhydride and succinic anhydride in the presence of a combination of (c) an aliphatic carboxylic acid and (d) an alkali metal carboxylate.

3. The process of claim 1 wherein the combination of water and the reaction product mixture is subjected to a shear rate of at least 1500 s −1 .

4. The process of claim 3 wherein the combination of water and the reaction product mixture is subjected to a shear rate of at least 3000 s −1 .

5. The process of claim 3 wherein the combination of water and the reaction product mixture is subjected to a shear rate of at least 8000 s −1 .

6. The process of claim 5 wherein shearing is conducted in a shear device running at a tip speed of at least 8 m/s.

7. The process of claim 6 wherein the reaction product mixture is contacted with 12 to 50 weight parts of water per weight part of hydroxypropyl methyl cellulose.

8. The process of claim 1 wherein shearing is conducted in a shear device running at a tip speed of at least 4 m/s.

9. The process of claim 8 wherein shearing is conducted in a shear device running at a tip speed of at least 8 m/s.

10. The process of claim 1 wherein the reaction product mixture is contacted with 12 to 300 weight parts of water per weight part of hydroxypropyl methyl cellulose.

11. The process of claim 1 wherein the reaction product mixture is contacted with water in a weight ratio [water/reaction product mixture excluding water] of from 1.0/1.0 to 5.0/1.0.

12. The process of claim 1 wherein the reaction product mixture is contacted with water in a weight ratio [water/aliphatic carboxylic acid] of from 3/1 to 30/1.

13. A process of preparing a hydroxypropyl methyl cellulose acetate succinate in the form of a powder wherein (a) a hydroxypropyl methyl cellulose is reacted with (b) acetic anhydride and succinic anhydride in the presence of (c) an aliphatic carboxylic acid and the hydroxypropyl methyl cellulose acetate succinate is precipitated from the reaction product mixture according to the process of claim 1 .

14. The process of claim 13 wherein a hydroxypropyl methyl cellulose acetate succinate is produced in the presence of (c) a combination of an aliphatic carboxylic acid and (d) an alkali metal carboxylate and wherein after the esterification reaction the hydroxypropyl methyl acetate succinate is precipitated from the reaction product mixture by contacting the reaction product mixture and water at a weight ratio [water/(total weight of (a) hydroxypropyl methyl cellulose, (b) acetic anhydride and succinic anhydride, (c) aliphatic carboxylic acid and (d) esterification catalyst)] of from [1.4/1.0] to [5.0/1.0].

15. The process of claim 1 wherein the product mixture is contacted with 12 to 400 weight parts of water per weight part of hydroxypropyl methyl cellulose.

Assignees

• Dow Global Technologies Llc

Inventors

• Sprehe Matthias
• Petermann Oliver
• Appell Robert B

Classifications

• C08B13/00 Primary

  Preparation of cellulose ether-esters · CPC title

• C08B11/20

  Post-etherification treatments of chemical or physical type, {e.g. mixed etherification in two steps}, including purification · CPC title