Propylene polymerization process
A technology of propylene and complexes, applied in the field of propylene polymerization, which can solve the problems of poor color stability, reduced aging performance, and high residual transition metals
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Embodiment 1
[0044] Example 1 [1,2-b] indenoindolyl complex 4 with open structure
[0045] (a), the preparation of indeno[1,2-b]indole 1
[0046] A mixture of 1-indanone (30.6 g, 232 mmol) and p-tolylhydrazine hydrochloride (37.0 g, 233 mmol) in ethanol (350 mL) and aqueous hydrochloric acid (12N, 18 mL) was heated to reflux for 90 minutes . The mixture was then cooled, filtered and the solid washed with ethanol (600 mL), followed by 20% aqueous ethanol (400 mL) and finally hexane (200 mL). The resulting beige solid was dried under vacuum (36.5 g 72%).
[0047] (b), N-methylation of 1
[0048] Product 1 (36.5 g, 166 mmol), aqueous NaOH (112 mL, 20 M, 2.2 mol), C 16 h 33 NMe 3 A mixture of Br (0.65 g, 1.78 mmol) and toluene (112 ml) was stirred vigorously, a solution of iodomethane (17.0 ml, 273 mmol) in toluene (15 ml) was added dropwise, and the mixture was stirred again at room temperature 4 hours, 3 hours at reflux. Upon cooling a crystalline solid formed which was filtered off ...
Embodiment 2
[0055] Open structure [1,2-b]indenoindolyl complex 5
[0056]Except that tert-butyramide lithium is replaced by 1,1,3,3-tetramethylbutyramide lithium, the synthesis steps of Example 1 are followed to obtain the open structure [1,2-b]indenoindolyl complex Object 5:
[0057]
Embodiment 4
[0063] Propylene polymerization
[0064] By mixing 5 mg of the open structure [1,2-b]indenoindolyl complex 4 prepared in Example 1 with 3.5 ml of MAO (10 wt% methylalumoxane in toluene) and 16.5 ml of toluene, in Prepare the solution of the complex and the activator in an inert atmosphere drying oven. The solution was aged for 30 minutes before being added to the polymerization reactor.
[0065] At room temperature, 400 ml of dry, oxygen-free propylene was added to a 1 liter stirred stainless steel reactor. Then 1.6 ml of a 25% by weight solution of triisobutylaluminum in heptane was flushed into the reactor with 50 ml of isobutane. The reactor was warmed to 50°C and equilibrated. A solution of 1.0 ml of complex and activator was then flushed into the reactor with 50 ml of isobutane to initiate polymerization. After 60 minutes of polymerization at 50°C, the reactor vent was opened to vent residual propylene and isobutane. The polymer was removed from the reactor, soaked o...
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