Olefin polymerization activators
A technology of olefin polymerization and metal activator, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, chemical instrument and method, etc. , increase power loss, etc.
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[0209] Examples 1-2 are the synthesis procedure of the intermediate of Activator 1, and Example 3 is the synthesis procedure of Activator 1. Examples 4-6 are synthetic procedures of intermediates of Activator 2, and Example 7 is a synthetic procedure of Activator 2. Example 8 is a synthetic procedure for an intermediate of Activator 3, and Example 9 is a synthetic procedure for Activator 3. In Example 10, various activators were used to synthesize polymer resins. The polymer resin characteristics were measured and reported in Tables 1-7. One or more features of the present disclosure are illustrated with the aid of the following examples:
example 1
[0210] Example 1: Synthesis of Activator 1 Precursor - Synthesis of Lithium Tetrakis(pentafluorophenyl)aluminate
[0211]
[0212] In a nitrogen filled glove box, a 100 mL round bottom flask was charged with bromopentafluorobenzene (1.0 mL, 8.02 mmol, 4 equiv) and diethyl ether (17 mL). The vessel was sealed with a septum, removed from the glove box, and attached to a nitrogen-filled Schlenk line. The reaction was cooled in a dry ice / isopropanol bath for 2 hours. A 1.65M solution of n-BuLi in hexane (4.86 mL, 8.02 mmol, 4.0 equiv) was added dropwise. The reaction was stirred at -78°C for 20 minutes. Add AlCl via syringe 3 (267.4 mg, 2.00 mmol, 1 eq) in diethyl ether (5.5 mL). Rinse the AlCl with additional ether (5.5 mL) 3 solution vial and add it to the solution. The solution was slowly warmed to room temperature and stirred for a total of 18 hours, forming a solid that went into solution. Transfer the suspension back to the glove box. Pass the suspension through a...
example 2
[0214] Example 2: Synthesis of Activator 1 Countercation: Synthesis of Armeenium M2HT Chloride
[0215]
[0216] In a nitrogen-filled glove box, Armeen M2HT (di-hydrogenated tallow alkylmethylamine (5.36 g, 10.0 mmol, 1 eq) available from AkzoNobel) was dissolved in hexane (150 mL). 2M HCl in ether (5.0 mL, 10.0 mmol, 1 eq) was slowly added dropwise to the stirred amine solution, causing immediate precipitation of a white solid. The suspension was stirred at room temperature for 15 minutes. The precipitated solid was bulky and fine, resulting in a viscous, gel-like suspension. Attempts were made to filter the suspension, however, it did not pass through the filter. The suspension was transferred back to the glass bottle and dried in vacuo to yield 4.76 g of white solid, 83% yield.
[0217] 1 H NMR (400MHz, toluene-d 8 )δ13.02-12.71 (m, 1H), 2.90 (dtd, J = 43.2, 12.4, 6.8Hz, 4H), 2.67 (d, J = 4.7Hz, 3H), 1.72 (ddt, J = 50.3, 13.3, 6.7Hz, 4H), 1.32(d, J=22.5Hz, 60H), 0....
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