US 11,890,896 B2
Preparation method of itaconate-butadiene bio-based engineering rubber
Liqun Zhang, Beijing (CN); Xinxin Zhou, Beijing (CN); Runguo Wang, Beijing (CN); Weiwei Lei, Beijing (CN); He Qiao, Beijing (CN); Kuo-chih Hua, Akron, OH (US); Joseph Kulig, Akron, OH (US); and Surendra K Chawla, Akron, OH (US)
Assigned to BEIJING UNIVERSITY OF CHEMICAL TECHNOLOGY, Beijing (CN); and THE GOODYEAR TIRE & RUBBER COMPANY, Akron, OH (US)
Appl. No. 15/736,198
Filed by Beijing University of Chemical Technology, Beijing (CN); and The Goodyear Tire & Rubber Company, Akron, OH (US)
PCT Filed Jun. 2, 2016, PCT No. PCT/CN2016/084508
§ 371(c)(1), (2) Date Mar. 27, 2018,
PCT Pub. No. WO2016/202175, PCT Pub. Date Dec. 22, 2016.
Claims priority of application No. 201510331148.8 (CN), filed on Jun. 15, 2015.
Prior Publication US 2018/0250984 A1, Sep. 6, 2018
Int. Cl. B60C 1/00 (2006.01); C08F 2/22 (2006.01); C08F 236/06 (2006.01); C08F 222/14 (2006.01); C08F 222/16 (2006.01); B65G 15/32 (2006.01); C08F 222/02 (2006.01); C08F 222/12 (2006.01); C08F 2/26 (2006.01); C08F 222/04 (2006.01)
CPC B60C 1/0016 (2013.01) [B60C 1/00 (2013.01); B65G 15/32 (2013.01); C08F 2/22 (2013.01); C08F 222/02 (2013.01); C08F 222/04 (2013.01); C08F 222/16 (2013.01); C08F 236/06 (2013.01); C08F 2500/01 (2013.01); C08F 2500/04 (2013.01)] 10 Claims
OG exemplary drawing
 
1. A method of preparing bio-based engineering rubber formed by emulsion polymerization of chemically crosslinked itaconate-butadiene copolymers, the method comprising:
A: performing the emulsion polymerization of itaconate and butadiene by:
mixing itaconate, emulsifier, electrolyte, activator and deionized water in a polymerization reactor,
closing the polymerization reactor,
removing air from the polymerization reactor using vacuum-pumping,
filling the polymerization reactor with nitrogen,
repeating mixing, closing, removing and filling operations for 1-5 times,
adding butadiene, deoxidant, and initiator to the polymerization reactor and performing reaction for 5-15 hours in the polymerization reactor under 1-20° C., 0.1-5 Mpa,
adding a terminator to terminate the reaction and performing demulsification and drying of the terminated reaction via an addition of a demulsifier to obtain a bio-based engineering elastomer raw glue comprising the itaconate-butadiene copolymers, wherein a mass ratio of the itaconate, the butadiene, the emulsifier, the electrolyte, the activator, the deoxidant and the initiator, the terminator and the deionized water is: 100: 1-100:1-10:0.1-5:0.01-5:0.1-5:0.01-5: 1-10:100-1000, a number average molecular weight of the itaconate-butadiene copolymers is about 53000-1640000, a weight-average molecular weight of the itaconate-butadiene copolymers is about 110000-2892000, and a molecular formula of itaconate is:

OG Complex Work Unit Chemistry
 wherein R1 and R2 are H or C1-10 alkyl, and R1 R2 are same or different; and
B: performing vulcanization process based on the obtained bio-based engineering elastomer using sulfur as a cross-linking agent in a sulfur vulcanizing system under 140-160° C. to prepare the bio-based engineering rubber comprising the itaconate-butadiene copolymers.