IP Library Granted Patent US 10,730,206
Granted Patent B2
US 10,730,206 · App. 15/543,156 · Granted Aug 4, 2020

Process for forming thermoplastic vulcanizates and thermoplastic vulcanizates made therefrom

Inventors: Declan Whelan (Rugby, GB); Stephen F. Roche (CWMBRAN Torfaen, GB); Porter C. Shannon (Seabrook, TX)
Assignee: ExxonMobil Chemical Patents Inc.
B29C35/02C08K3/16C08L23/12C08L23/14C08L23/16
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Quick Facts
Patent No.
US 10,730,206
App. No.
15/543,156
Granted
Aug 4, 2020
Kind
B2
Abstract

Provided are methods for producing a thermoplastic vulcanizate and thermoplastic vulcanizates provided therein. The method includes introducing vulcanizable rubber, thermoplastic resin, a masterbatch of a propylene-based elastomer and a cure accelerator for a phenolic resin curative to the reactor, and phenolic resin curative to a reactor and dynamically vulcanizing the rubber with the phenolic resin curative in the presence of the cure accelerator and the thermoplastic resin.

Claims (25)

1. A composition comprising propylene-based elastomer and from about 10 wt % to about 90 wt % stannous chloride, based on the weight of the composition, where the propylene-based elastomer comprises propylene-derived units and 5 to 30 wt % of α-olefin-derived units and where the propylene-based elastomer has a melting temperature of less than 120° C. and a heat of fusion of less than 75 J/g.

2. A process for making a thermoplastic vulcanizate comprising the composition of claim 1 , the process comprising:

(a) introducing a vulcanizable rubber to a reactor;

(b) introducing a thermoplastic resin to the reactor;

(c) introducing a masterbatch comprising the composition of claim 1 to the reactor;

(d) introducing a phenolic resin curative to the reactor; and

(e) dynamically vulcanizing the vulcanizable rubber with the phenolic resin curative in the presence of the masterbatch and the thermoplastic resin.

3. The method of claim 2 , wherein the step of vulcanizing occurs at a temperature above the melt temperature of the thermoplastic resin.

4. A method for making a thermoplastic vulcanizate comprising the composition of claim 1 , the method comprising:

(a) mixing a vulcanizable rubber and a thermoplastic resin above the melt temperature of the thermoplastic resin to form a molten mass;

(b) adding a masterbatch comprising the composition of claim 1 to the molten mass;

(c) melting the propylene-based elastomer of the masterbatch to thereby disperse stannous chloride within the molten mass;

(d) adding a phenolic curative to the molten mass; and

(e) dynamically vulcanizing the vulcanizable rubber with the phenolic resin in the presence of the stannous chloride.

5. The method of claim 2 , where the masterbatch comprises from about 10 wt % to about 70 wt % stannous chloride based on the total weight of the masterbatch.

6. The method of claim 2 , wherein the masterbatch contains less than 25 wt % of material other than the stannous chloride and the propylene-based elastomer.

7. The method of claim 2 , wherein the masterbatch contains less than 5 wt % of material other than the stannous chloride and the propylene-based elastomer.

8. The method of claim 2 , wherein the masterbatch contains less than 1 wt % of material other than the stannous chloride and the propylene-based elastomer.

9. The method of claim 2 , wherein the masterbatch consists essentially of the stannous chloride and the propylene-based elastomer.

10. The method of claim 2 , wherein the masterbatch is charged to the reactor in the form of pellets.

11. The method of claim 2 , wherein the thermoplastic resin comprises polypropylene.

12. The method of claim 2 , wherein the vulcanizable rubber comprises ethylene-α-olefin-diene copolymer.

13. A method for making a thermoplastic vulcanizate comprising the composition of claim 1 , the method comprising steps of:

adding a ethylene-propylene-diene copolymer to a twin-screw extruder through the feed throat of the extruder; adding polypropylene to the twin-screw extruder through the feed throat of the extruder; mixing, within an initial mix zone, the ethylene-propylene-diene copolymer and the polypropylene at a temperature above the melt temperature of the polypropylene to form a molten mass; charging pellets that include the composition of claim 1 to the twin-screw extruder through an inlet in a barrel downstream of the initial mix zone;

heating the pellets above the melt temperature of the propylene-based elastomer and mixing the molten pellets with the molten mass; charging a phenolic resin curative to the twin-extruder through an inlet in a barrel downstream of the barrel where the pellets are charged; mixing the phenolic resin with the molten mass while transferring the molten mass through a cure zone where dynamic vulcanization of the ethylene-propylene-diene copolymer takes place to thereby form a thermoplastic vulcanizate; removing the thermoplastic vulcanizate from the twin-screw extruder; cooling the thermoplastic vulcanizate; and pelletizing the thermoplastic vulcanizate.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 25, 2022
From: EXXONMOBIL CHEMICAL PATENTS INC.
To: SANTOPRENE PRODUCTION PENSACOLA LLC
Reel/Frame 059248/0456 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 25, 2022
From: SANTOPRENE PRODUCTION PENSACOLA LLC
To: CELANESE INTERNATIONAL CORPORATION
Reel/Frame 059248/0673 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 11, 2017
From: WHELAN, DECLAN; ROCHE, STEPHEN F.; SHANNON, PORTER C.
To: EXXONMOBIL CHEMICAL PATENTS INC.
Reel/Frame 043837/0028 →
Continuity (2)
Provisional Application 62121223 · Feb 26, 2015
Related Publication 20180009135A1 · Jan 11, 2018