Ethylene → HCID 131723574, compound

Temperature

70 °C

The following polymerization procedure was utilized in all of the examples. First, varying amounts of 86 to 98 wt % DCPD in toluene were charged to a dry, 1 gallon reactor, which was then heated to 70° C. The specific amounts of DCPD used are specified in Table 1. In Examples 1-10, 200 milliliters of polymerization grade toluene were charged to the reactor; however in Examples 11-12, the 200 milliliters of toluene were not added. Then, the reactor was pressured to 150 psig with ethylene and then depressured. This pressure/depressure cycle was completed three times. Ethylene was then charged to maintain a pressure of 100 psig in the reactor. Then, the ethylene pressure was increased to 300 psig and maintained for 15 minutes while the reactor was stirred. The ethylene flow was then stopped, and the reactor was vented to 50 or 100 psig. 10-30 milliliters of 10 wt % methylaluminoxane (MAO) in toluene and 0.01 to 0.04 grams of a titanium complex were then charged to the reactor. The ethylene flow to the reactor was re-established at between 50 and 300 psig and maintained for between 60 to 90 minutes to produce an ethylene/dicyclopentadiene polymer mixture comprising ethylene/dicyclopentadiene polymer, toluene, and unreacted ethylene and DCPD. The ethylene flow was then stopped by adding 5 milliliters of methanol, and the reactor was allowed to cool. The ethylene/dicyclopentadiene polymer mixture was then washed and dried in a vacuum oven at 50° C. In some examples, 5 milliliters of an antioxidant solution were also added to the ethylene/dicyclopentadiene polymer mixture prior to drying. The antioxidant solution contained 10 weight percent tris(p-nonylphenyl) phosphite (TNPP) and 40 weight percent tetrakis(methylene(3,5-di-tert-butyl-4-hydroxyhydrocinnamate in cyclohexane. The TNPP was obtained from GE Specialty Chemicals in Parkersburg, W.Va. The tetrakis(methylene(3,5-di-tert-butyl-4-hydroxyhydrocinnamate was obtained as Irganox® 1076 from Ciba-Geigy Corporation in Hawthorne, N.Y.

1. customThe following polymerization procedure
2. additionwere charged to a dry, 1 gallon reactor, which
3. additionwere charged to the reactor
4. temperatureto maintain a pressure of 100 psig in the reactor
5. temperaturemaintained for 15 minutes while the reactor
6. temperaturemaintained for between 60 to 90 minutes

ORD record

ord-e7b54051cdaa41dba35d8c2bb435db50

Source dataset

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06469117B1