4-tert-Butylcatechol → Isoprene butadiene

In this example, a coupled isoprene-butadiene rubber (IBR) was prepared in a one-gallon (3.8 liters) batch reactor at 70° C. In the procedure used, 2,000 grams of a silica/molecular sieve/aluminum dried premix containing 19.0 weight percent of a mixture of isoprene and 1,3-butadiene in hexanes at the ratio of 10:90 was charged into a one-gallon (3.8 liters) reactor. After the amount of impurity in the premix was determined, 4.0 ml of a 1.0 M solution of n-butyl lithium (in hexane) was added to the reactor. The target Mn (number averaged molecular weight) was 100,000. The polymerization was allowed to proceed at 70° C. for three hours. An analysis of the residual monomer indicated that monomers was all consumed. Then, 1.0 ml of a 1 M solution of tin tetrachloride (in hexane) was added to the reactor and the coupling reaction was carried out at the same temperature for 30 minutes. At this time, 1.5 phr (parts per 100 parts by weight of rubber) of 4-t-butylcatechol and 0.5 phr of TMEDA was added to the reactor to shortstop the polymerization and to stabilize the polymer.

1. dry with material2,000 grams of a silica/molecular sieve/aluminum dried
2. additionpremix
3. additioncontaining
4. addition19.0 weight percent of a mixture of isoprene and 1,3-butadiene in hexanes at the ratio of 10:90
5. additionwas charged into a one-gallon (3.8 liters) reactor
6. addition4.0 ml of a 1.0 M solution of n-butyl lithium (in hexane) was added to the reactor
7. additionThen, 1.0 ml of a 1 M solution of tin tetrachloride (in hexane) was added to the reactor
8. customthe coupling reaction
9. waitwas carried out at the same temperature for 30 minutes
10. customthe polymerization

ORD-Eintrag

ord-d9cab5a4ea6841a088ee1bc33665e002

Quelldatensatz

uspto-grants-2001_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06271317B1