Ethylene oligomerization catalyst, preparation method and application
An ethylene oligomerization and catalyst technology, applied in the field of ethylene oligomerization catalyst and preparation, can solve the problems of low oligomerization activity and achieve the effects of good ethylene dimerization and trimerization selectivity and high reaction activity
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[0012] The preparation method of catalyst of the present invention comprises the steps:
[0013] (1) benzoyl chloride derivatives shown in formula (II) are dissolved in tetrahydrofuran to make a solution, 2-aminopyridine derivatives shown in formula (III) are dissolved in pyridine to make a solution, and then described tetrahydrofuran The solution is added to the pyridine solution, and the compound of formula (II) and formula (III) is fully reacted at 20-100°C in a molar ratio of 1-1.1:1, then washed with water, and the solvent is removed to obtain N-pyridylbenzamides Ligand compound, in said formula (II), formula (III), R 1 , R 2 Respectively selected from hydrogen, C 1 ~C 4 Alkyl or nitro,
[0014]
[0015] (2) N-pyridylbenzamide ligand compound is reacted with sodium hydride in a molar ratio of 1:1.0 to 1.5 in the presence of an organic medium, and then added toluene and trans - Chloride (alkaryl) (triphenylphosphine) nickel to continue the reaction, then filter, af...
example 1
[0026] Preparation of trans-(phenyl)(triphenylphosphine)nickel chloride.
[0027] Under nitrogen flow, 125 grams (0.4883mol) of triphenylphosphine (Beijing Reagent Factory) and 21.3 grams (0.083mol) of anhydrous diacetylacetonate nickel (STREM company) were suspended in 800 milliliters of ether, and the mixture was washed with ice-methanol The bath was cooled to 0°C, and 100 ml of ether solution containing 28 g of triethylaluminum was slowly added dropwise. During the dropwise addition, the reaction mixture turned from green to brick red and a reddish-brown precipitate formed. After the dropwise addition, stir at 5-10°C for 30 minutes, then stir at 25°C for 2 hours, filter the precipitate, wash twice with 40 milliliters of ether, and vacuum-dry at 25°C for 4 hours to obtain 81.2 grams of tetrakis(triphenylphosphine)nickel. The melting point is 123-128°C.
[0028]Under the protection of nitrogen, suspend 0.9 g (0.81 mmol) of tetrakis(triphenylphosphine) nickel in 10 ml of tol...
example 2
[0030] Prepare tetrakis(triphenylphosphine)nickel according to the method of example 1, the crude product obtained after washing and drying with ether is dissolved at 60°C with 400 milliliters of benzene containing 40 grams of triphenylphosphine, and 200 Milliliter of heptane, filtered, and the resulting solid was washed twice with 200 milliliters of heptane and 180 milliliters of ether. Repeat the above operations to obtain reddish-brown crystals, which were dried at 90°C under reduced pressure for 16 hours to obtain 50 g of pure tetrakis(triphenylphosphine)nickel with a melting point of 123-128°C.
[0031] Under the protection of nitrogen, suspend 0.9 g (0.81 mmol) tetrakis (triphenylphosphine) nickel in 10 ml of toluene, add 0.83 mmol of chlorinated naphthalene at 20 ° C, and stir for 20 minutes to obtain a uniform solution. The red color disappeared, and yellow-brown crystals were precipitated. The crystals were filtered out, washed with 10 ml of petroleum ether, and dried...
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