Binuclear nickel-series olefine oligomerization catalyst, and its preparation method and use
A technology for catalysts and olefins, which is applied in the field of binuclear nickel-based olefin oligomerization catalysts, production methods and applications, which can solve the problems of low ligand yield, low oligomerization activity, and difficulty in complete completion, and achieve high activity and good yield Effect
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[0016] The preparation method of catalyst of the present invention comprises:
[0017] (1) In a non-polar organic solvent, using an organic acid as a catalyst, the carbonylpyridine compound represented by the formula (II) and the bridged phenylenediamine compound represented by the formula (III) are heated at 20 to 150° C. Carry out the condensation reaction at a molar ratio of 2:1, remove the solvent, and dry the resulting solid to obtain the ligand compound,
[0018]
[0019] In said formula (II), R 4 is a substituent on the pyridine ring, the number of which is 1 to 4, R 4 selected from hydrogen or C 1 ~C 6 the alkyl group, R 3 selected from hydrogen or C 1 ~C 4 The alkyl group; in formula (III), R 1 and R 2 are the substituents on the benzene ring, the number of substituents on each benzene ring is 1 to 4, R 1 and R 2 respectively selected from hydrogen or C 1 ~C 8 The alkyl group, Y is selected from -O-, -S-, -CH 2 -;
example 1
[0031] Prepare the catalyst {bis[pyridinecarbaldehyde] acetal 4,4'-methylenebis(2,6-diethylaniline)} nickel dibromide.
[0032] (1) Preparation of Ligand Compounds
[0033] In a three-neck flask with a reflux condenser, add 10 milliliters of toluene and 0.005 moles of 4,4'-methylene-bis(2,6-diethylaniline) and 0.01 moles of 2-pyridinecarbaldehyde, drop into 2 Drop formic acid, stir and react at 60°C for 4 hours, let the reactant stand at -10°C for 48 hours, add 10 ml of hexane, filter, wash the solid with 10 ml of hexane twice, and dry under reduced pressure at 60°C for 1 hour. 2.35 g of white solid was obtained, which was ligand compound a: bis[pyridinecarbaldehyde] acetal 4,4'-methylene-bis(2,6-diethylaniline), yield 96% by mass,
[0034] Elemental analysis measured (calculated), mass %: C80.98 (81.11); H7.51 (7.43); N11.35 (11.46).
[0035] Infrared spectrum characteristic peak, cm -1 : 1630.70; 1578.94; 1562.60.
[0036] h 1 NMR: δ7.05; δ4.05; δ8.78; δ7.26-8.38.
[00...
example 2
[0043] Preparation of {bis[pyridinecarbaldehyde] acetal 4,4'-methylene-bis(2,6-diisopropylaniline)}nickel dibromide.
[0044] (1) Preparation of ligand compounds: prepare ligands according to the method of example 1 (1), differently use 4,4'-methylene-bis(2,6-diisopropylaniline) containing 0.005 moles and 0.01 Moles of 2-pyridinecarbaldehyde are subjected to condensation reaction, and the non-polar organic solvent used in the reaction is 10 milliliters of benzene to obtain ligand compound b: bis[pyridinecarbaldehyde] acetal 4,4'-methylene-bis(2,6-diiso Propylaniline), yield 98% by mass.
[0045] Elemental analysis measured (calculated), mass %: C81.18 (81.57); H8.13 (8.14); N10.26 (10.29).
[0046] Infrared spectrum characteristic peak, cm -1 : 1635.70; 1584.94; 1567.60.
[0047] h 1 NMR: δ7.02; δ4.02; δ8.74; δ7.26-8.38.
[0048] (2) Preparation of catalyst
[0049] Prepare catalyst by example 1 (2) step method, difference is with ligand b and NiBr 2 DME reaction to ob...
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