IP Library Granted Patent US 11,161,970
Granted Patent B2
US 11,161,970 · App. 16/065,457 · Granted Nov 2, 2021

Saponified ethylene-vinyl ester-based copolymer composition and producing method therefor

Inventors: Nobuaki Sato (Osaka, JP); Taiji Kanda (Osaka, JP); Ayano Nakashima (Osaka, JP)
Assignee: MITSUBISHI CHEMICAL CORPORATION
C08L29/04C08K3/38C08K5/098C08K2003/387
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Quick Facts
Patent No.
US 11,161,970
App. No.
16/065,457
Granted
Nov 2, 2021
Kind
B2
Abstract

The purpose of the present invention is to provide: an EVOH resin-based composition (pellet) which has a desired melt viscosity without increasing the boron content, thereby being effective for surging prevention; and a method for producing the resin composition. The EVOH-based resin composition contains a boric acid compound and the boric acid compound contains tetracoordinated boron. An EVOH-based resin paste containing a boric acid compounds is brought into contact with an aqueous solution containing a boric acid compound and alkali metal salt at an elevated temperature and an elevated pressure so that the amount of alkali metal salt is from 300 to 1000 ppm based on the EVOH-based resin paste, thereby converting the boron of the boric acid compound to tetracoordinated structure.

Claims (26)

1. A resin composition comprising a saponified ethylene-vinyl ester-based copolymer and a boric acid,

wherein the resin composition contains tetracoordinated boron, and

wherein a percentage of the tetracoordinated boron in the boric acid is from 10 to 99% by mol based on the boric acid.

2. The resin composition according to claim 1 , wherein the amount of the boric acid is in the range of 1 to 350 ppm in terms of boron based on the saponified ethylene-vinyl ester-based copolymer.

3. The resin composition according to claim 1 , further comprising 300 to 1000 ppm of an alkali metal salt in terms of metal per the saponified ethylene-vinyl ester-based copolymer.

4. The resin composition according to claim 3 , wherein the alkali metal salt is a sodium salt.

5. The resin composition according to claim 3 , wherein the amount of the alkali metal salt per the boric acid is an amount such that a ratio in weight of alkali metal salt in terms of alkali metal to the boric acid compound in terms of boron is from 0.8 to 10.

6. The resin composition according to claim 1 , wherein a tensile viscosity at a tensile strain rate of 100 sec -1 at 210° C. is in the range of 1.0×10 2 to 1.0×10 6 Pa·s.

7. A method for producing a saponified ethylene-vinyl ester-based copolymer composition containing tetracoordinated boron comprising,

contacting a saponified ethylene-vinyl ester-based copolymer paste comprising a first boric acid compound with an aqueous solution containing a second boric acid compound and an alkali metal salt under an elevated temperature and pressure condition to convert at least a part of boron in the first boric acid compound contained in the paste to tetracoordinated boron,

wherein the aqueous solution contains the second boric acid compound and an alkali metal salt at respective content such that the resulting total content of the first boric acid compound and the second boric acid compound is from 1 to 350 ppm in terms of boron per saponified ethylene-vinyl ester-based copolymer in the saponified ethylene-vinyl ester-based copolymer composition and the content of the alkali metal salt is from 300 to 1000 ppm in terms of metal per saponified ethylene-vinyl ester-based copolymer in the saponified ethylene-vinyl ester-based copolymer composition.

8. The producing method according to claim 7 , wherein the conversion process is carried out in a system having a temperature of 50 to 150° C. and a pressure of 0.01 to 1 MPaG as a difference between a pressure in the system and air pressure.

9. The producing method according to claim 7 , wherein the contact is carried out with kneading the saponified ethylene-vinyl ester-based copolymer paste with the aqueous solution.

10. The producing method according to claim 7 , wherein the saponified ethylene-vinyl ester-based copolymer paste contains 1 to 350 ppm of the first boric acid compound in terms of boron per the saponified ethylene-vinyl ester-based copolymer, and contains 1000 to 4000 ppm of the alkali metal salt in terms of metal per the saponified ethylene-vinyl ester-based copolymer.

11. The producing method according to claim 7 , wherein the aqueous solution

contains the second boric acid compound in a concentration of 1 to 50 ppm in terms of boron, and

contains the alkali metal salt in a concentration of 50 to 1500 ppm in terms of metal.

12. A resin composition comprising a saponified ethylene-vinyl ester-based copolymer and a boric acid,

wherein the resin composition contains tetracoordinated boron;

wherein the tetracoordinated boron is a result of contacting a paste comprising the saponified ethylene-vinyl ester-based copolymer comprising a first boric acid compound with an aqueous solution containing a second boric acid compound and an alkali metal salt under an elevated temperature and pressure condition to convert at least a part of boron in the first boric acid compound contained in the paste to tetracoordinated boron.

13. The resin composition according to claim 12 , wherein the amount of the boric acid is in the range of 1 to 350 ppm in terms of boron based on the saponified ethylene-vinyl ester-based copolymer.

14. The resin composition according to claim 12 , wherein a percentage of the tetracoordinated boron in the boric acid is from 10 to 99% by mol based on the boric acid.

15. The resin composition according to claim 12 , comprising 300 to 1000 ppm of the alkali metal salt in terms of metal per the saponified ethylene-vinyl ester-based copolymer.

16. The resin composition according to claim 15 , wherein the alkali metal salt is a sodium salt.

17. The resin composition according to claim 15 , wherein the amount of the alkali metal salt per the boric acid is an amount such that a ratio in weight of alkali metal salt in terms of alkali metal to the boric acid compound in terms of boron is from 0.8 to 10.

18. The resin composition according to claim 12 , wherein a tensile viscosity at a tensile strain rate of 100 sec 1 at 210° C. is in the range of 1.0×10 2 to 1.0×10 6 Pa·s.

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 Sep 21, 2018
From: SATO, NOBUAKI; KANDA, TAIJI; NAKASHIMA, AYANO
To: THE NIPPON SYNTHETIC CHEMICAL INDUSTRY CO., LTD.
Reel/Frame 046935/0584 →