IP Library Granted Patent US 11,401,355
Granted Patent B2
US 11,401,355 · App. 15/913,069 · Granted Aug 2, 2022

Ethylene-vinyl alcohol copolymer, method of producing ethylene-vinyl alcohol copolymer, resin composition, and multilayer structure

Inventors: Tomonori Yoshida (Osaka, JP); Nobuaki Sato (Osaka, JP); Masahiko Taniguchi (Osaka, JP)
Assignee: MITSUBISHI CHEMICAL CORPORATION
C08F8/16B32B27/28C08F8/12C08F210/02C08F216/06C08F2800/10C08F2810/40
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Quick Facts
Patent No.
US 11,401,355
App. No.
15/913,069
Granted
Aug 2, 2022
Kind
B2
Abstract

An ethylene-vinyl alcohol copolymer has an ethylene content of 20 to 60 mol % and includes a carboxylic acid group and a lactone ring group present at terminals thereof, wherein the molar concentration (Y/Z) of a lactone ring molar content (Y) to a sum (Z) of a carboxylic acid molar content (X) and the lactone ring molar content (Y) is not less than 58 mol %. The ethylene-vinyl alcohol copolymer is excellent in high-temperature thermal stability substantially without thermal decomposition, and is free from odor emanation and coloration even if being processed at a higher temperature.

Claims (25)

1. A method of producing an ethylene-vinyl alcohol copolymer comprising

an ethylene unit and a vinyl alcohol unit as monomer units, and

a carboxylic acid group and a lactone ring group present at terminals thereof,

wherein a molar concentration (Y/Z) of a lactone ring molar content (Y) to a sum (Z) of a carboxylic acid molar content (X) and the lactone ring molar content (Y) is not less than 63 mol %,

the method comprising:

[I] saponifying an ethylene-vinyl ester copolymer to provide an ethylene-vinyl alcohol copolymer intermediate product;

[II] chemically treating the ethylene-vinyl alcohol copolymer intermediate product with a chemical treatment liquid; and

[III] drying the chemically treated ethylene-vinyl alcohol copolymer intermediate product;

wherein a monovalent carboxylic acid concentration of the chemical treatment liquid is 1 to 50000 ppm in the chemical treatment [II];

wherein a weight-based ratio of the monovalent carboxylic acid concentration to a metal ion concentration (monovalent carboxylic acid concentration/metal ion concentration) is 13 to 100 in the chemical treatment liquid in the chemical treatment [II]; and

wherein the metal ion in the chemical treatment liquid is a metal ion of carboxylic acid metal salt.

2. The ethylene-vinyl alcohol copolymer production method according to claim 1 , wherein the chemical treatment [II] of chemically treating the ethylene-vinyl alcohol copolymer intermediate product with the chemical treatment liquid includes preparing a plurality of chemical treatment liquids having different carboxylic acid concentrations, and chemically treating the ethylene-vinyl alcohol copolymer intermediate product with the respective chemical treatment liquids on multiple stages, wherein the weight-based ratio of the monovalent carboxylic acid concentration to the metal ion concentration (monovalent carboxylic acid concentration/metal ion concentration) is 13 to 100 in a chemical treatment liquid having the highest monovalent carboxylic acid concentration among the plurality of chemical treatment liquids.

3. The ethylene-vinyl alcohol copolymer production method according to claim 1 , wherein the drying [III] is performed at a drying temperature of 80° C. to 150° C.

4. An ethylene-vinyl alcohol copolymer comprising

an ethylene unit and a vinyl alcohol unit as monomer units, and

a carboxylic acid group and a lactone ring group present at terminals thereof,

wherein a molar concentration (Y/Z) of a lactone ring molar content (Y) to a sum (Z) of a carboxylic acid molar content (X) and the lactone ring molar content (Y) is not less than 63 mol %, and

wherein the ethylene-vinyl alcohol copolymer does not comprise a 1,2-diol structure at a side chain thereof.

5. The ethylene-vinyl alcohol copolymer production method according to claim 1 , wherein the ethylene-vinyl alcohol copolymer does not comprise a 1,2-diol structure at a side chain thereof.

6. The ethylene-vinyl alcohol copolymer according to claim 4 , wherein the sum (Z) of the carboxylic acid molar content (X) and the lactone ring molar content (Y) is 0.01 to 0.3 mol % based on a total amount of the monomer units of the ethylene-vinyl alcohol copolymer.

7. The ethylene-vinyl alcohol copolymer according to claim 4 , wherein the lactone ring molar content (Y) is 0.01 to 0.3 mol % based on a total amount of the monomer units of the ethylene-vinyl alcohol copolymer.

8. The ethylene-vinyl alcohol copolymer according to claim 4 , wherein the carboxylic acid molar content (X) is 0.01 to 0.3 mol % based on a total amount of the monomer units of the ethylene-vinyl alcohol copolymer.

9. A resin composition comprising the ethylene-vinyl alcohol copolymer according to claim 4 .

10. A multilayer structure comprising at least one layer comprising the ethylene-vinyl alcohol copolymer according to claim 4 .

11. A multilayer structure comprising at least one layer comprising the resin composition according to claim 9 .

Assignments (2)
MERGER Recorded May 2, 2019
From: THE NIPPON SYNTHETIC CHEMICAL INDUSTRY CO., LTD.
To: MITSUBISHI CHEMICAL CORPORATION
Reel/Frame 049110/0285 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 6, 2018
From: YOSHIDA, TOMONORI; SATO, NOBUAKI; TANIGUCHI, MASAHIKO
To: THE NIPPON SYNTHETIC CHEMICAL INDUSTRY CO., LTD.
Reel/Frame 045121/0956 →
Cited By (1)
US 12,583,208