Catalyst for olefin polymerization
A technology for olefin polymerization and catalysts, applied in the field of olefin polymerization catalysts, can solve the problems of low polymer activity and isotactic index, inability to produce, and increased hydrogen consumption
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Embodiment 1
[0051] Preparation of diol ester compound 2,4-pentanediol dibenzoate
[0052] (1) Preparation of 2,4-pentanediol
[0053] A mixture of 10g of 2,4-pentanedione and 30ml of methanol was added dropwise to a mixed solution of 2.5g of sodium borohydride, 0.1g of sodium hydroxide and 25ml of water at 0-10°C. After the addition, the solvent was removed under reduced pressure and extracted continuously with 40ml of ethyl acetate for 15h. The solvent was removed and column chromatography was used to obtain 2,4-pentanediol as a colorless liquid with a yield of 90%.
[0054] (2) Preparation of 2,4-pentanediol dibenzoate
[0055] Add 30ml tetrahydrofuran and 0.09mol pyridine to 0.03mol 2,4-pentanediol, add 0.075mol benzoyl chloride under stirring, and heat to reflux for 4h. After cooling, add 20ml of saturated brine, extract with ethyl acetate, anhydrous Na 2 SO 4 Dry and remove solvent. Column chromatography or distillation under reduced pressure gave 2,4-pentanediol dibenzoate as ...
Embodiment 2
[0058] 2A, the preparation of solid catalyst A (main catalyst)
[0059] Add 100ml of titanium tetrachloride to a 300ml stirred glass reaction bottle fully replaced by high-purity nitrogen, cool to -20°C, add spherical magnesium chloride alcoholate (see Chinese patent CN1330086A for the preparation method), and slowly raise the temperature in stages To 110°C, add 2.5mmol of 2,4-pentanediol dibenzoate and 3.9mmol of dibutyl phthalate prepared in Example 1 during the heating process, and filter at 110°C for 0.5h The liquid was treated twice by adding titanium tetrachloride, then washed five times with hexane, and dried in vacuum to obtain solid catalyst A (main catalyst).
[0060] 2B, propylene polymerization
[0061] In a 5-liter autoclave, a nitrogen stream was used to purge at 70° C. for 1 hour, then the polymerization vessel was replaced 3 times with gas-phase propylene, and 5 ml of a hexane solution of triethylaluminum (triethylaluminum) was introduced under nitrogen protec...
Embodiment 3～7
[0063] The solid catalyst prepared in 2A of Example 2 was polymerized according to the method of propylene polymerization in 2B of Example 2, and the amounts of hydrogen added were 1NL, 2NL, 4NL, 6NL, and 8NL. The external electron donor added during the polymerization is a hexane solution of tetraethoxysilane (TEOS). The polymerization and test results are shown in Table 1 and Table 2.
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