Electron donors for ziegler-natta precatalyst preparation and catalyst system for olefin polymerization
A technology of pre-catalyst and electron donor, applied in germanium-organic compounds, chemical instruments and methods, compounds of elements of group 4/14 of the periodic table, etc., can solve problems such as low catalyst activity
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Embodiment 1
[0173] Example 1: Preparation of an Exemplary Electron Donor
[0174] plan 1
[0175]
[0176] Preparation of electron donor 1. Electron donor 1 was prepared as shown in Scheme 1. Add cyclotetramethylenedichlorosilane (1.3 mL), chloroiodomethane (2.0 mL), THF (50 mL) to a Schlenk tube and cool to -78°C. MeLiLiBr (27 mL, 1.6M in hexane) was added dropwise over 30 minutes. The reaction solution was then warmed to room temperature over 1 hour. The resulting solution was treated with NH 4 Quenching with Cl solution and standard workup afforded intermediate 1,1-bis(chloromethyl)silacyclopentane as a colorless liquid. A round bottom flask was charged with DMF (40 mL), 1,1-bis(chloromethyl)silacyclopentane (1.6 g) and sodium benzoate (6 g) and stirred at 100° C. overnight. Electron donor 1 (4.2 g) was obtained after work-up as a colorless syrup.
[0177] Preparation of electron donor 2. A Schlenk tube was charged with cyclopentamethylenedichlorosilane (3.0 mL), chloroi...
Embodiment 2
[0186] Example 2. Exemplary Polymerization with Electron Donors. The prepared precatalyst was used in propylene polymerization conditions using the following exemplary method. The propylene polymerization was carried out in a one gallon reactor. The reactor was purged at 100°C for one hour under nitrogen. At room temperature, 1.5 ml of 25% by weight TEAl (triethylaluminum) in heptane was added to the reactor. Next, 0.94 ml of a 0.0768M solution of cyclohexylmethyldimethoxysilane (Donor C) was added to the reactor, followed by 7.0 mg of precatalyst as a 1 wt % hexane slurry. Charge the reactor with 5 standard liters of H 2 , and then charge 1300g of propylene. The reactor was heated to 70°C and held at this temperature for one hour. The polymerization reaction is quenched by venting the reactor, and the polymer is recovered.
[0187] A number of electron donors listed in Table 1 were similarly tested and the results are listed in Table 2. Ranges for CE, %XS and MFR are ...
Embodiment 3
[0195] Example 3. Exemplary Polymerization Using Electron Donor 4: A typical polymerization process was carried out in a reactor unit equipped with a magnetically coupled mechanical stirrer with a geometric volume of about 23 mL and a working volume of the liquid phase of about 5 mL. The unit was first purged at 90°C to 140°C for 8 hours under intermittent nitrogen flow. Cool the unit to room temperature and assemble a disposable 10 mL glass vial and a stirrer paddle. Then a certain amount of dry heptane was mixed with TEAl and H as scavengers through a syringe pump 2 (pH 2 varying from 0.03-0.2 bar) together were fed to the reactor system at a temperature of 70°C and an operating pressure of propylene (total reactor pressure of 5.5 bar). Under these conditions using the slurry needle system, a test amount of precatalyst (approx. 0.1 mg) in a heptane slurry and a solution of TEAl / additional external electron donor in heptane was injected into the cell by adding Propylene w...
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