Pretransistion metal catalytic system for ethene polymerisation and copolymerisation, its preparation method and uses
A technology for pre-transition metal and ethylene polymerization, which is applied in the field of pre-transition metal catalytic systems, can solve problems such as not being retrieved, and achieve the effects of reducing costs and improving the catalytic activity of ethylene polymerization and copolymerization.
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Embodiment 1
[0044] Complex (L1) 3 Zr 2 Cl4 Synthesis
[0045] (1) Synthesis of 4,4'-dimethyl-2,2'-propylene-bisphenol
[0046] Add 128ml (600mmol) of p-cresol and 8.8ml (60mmol) of n-propionaldehyde in a 250ml three-necked flask, stir, and add 8ml of concentrated hydrochloric acid dropwise when heated to 63°C, the solution immediately turns yellow, and the temperature rises to 85°C , maintain the reaction for 5 hours, it is an orange-red solution, distilled under reduced pressure, the residue is dissolved in a mixed solvent of 80ml chloroform: 80ml petroleum ether, after the precipitate is precipitated, the precipitate is filtered out, and vacuum-dried to obtain milky white 4,4'-di Methyl-2,2'-propylene-bisphenol product.
[0047] (2) Synthesis of 5,5'-dimethyl-3,3'-propylene-disalicylaldehyde
[0048] Under the protection of nitrogen, add 7.68g (30mmol) of 4,4'-dimethyl-2,2'-propylene-bisphenol synthesized above into a 250ml three-necked flask, dissolve with 60ml of refluxed benzene,...
Embodiment 2
[0069] Metal complexes (L2) 3 Zr 2 Cl 4 Synthesis
[0070] (1) Synthetic Ligand L2
[0071] Under a nitrogen atmosphere, add 0.51g (1.63mmol) of 5,5'-dimethyl-3,3'-propylene-disalicylaldehyde synthesized according to the method in Example 1 into a 250ml three-necked flask, and dissolve it in 40ml of methanol , and then add 0.45ml (3.91mmol) of cyclohexylamine and 0.2ml of formic acid, and stir at room temperature for 24 hours. The precipitate was filtered off and dried in vacuo to yield 0.48 g of Ligand L2 as a yellow powder.
[0072] Its structural formula is as follows:
[0073]
[0074] Ligand L2
[0075] EI—mass spectrum: 474M +
[0076] (2) Synthesis of metal complexes (L2) 3 Zr 2 Cl 4
[0077] Under a nitrogen atmosphere, add 0.55g (1.16mmol) of ligand L2 synthesized according to the method in Example 2 into a three-necked flask, add 30ml of tetrahydrofuran to dissolve, then cool down to below -70°C, and slowly add 1.05ml (1.62mmol) of n-butyl Lithium-bas...
Embodiment 3
[0081] (1) Take 4.0 grams of silica gel (Grace product) after high-temperature treatment (under nitrogen, roast at 400 ° C for 4 hours, and then vacuumize at 120 ° C for 16 hours) and join in a 250 ml reactor, add 30 ml of toluene and 25 Milliliter 10wt% MAO (methylaluminoxane) toluene solution, the a value of MAO was 20, was heated up to 50 ° C, stirred for 4 hours, then washed 5 times with 50 ml of toluene, vacuum dried to obtain a white solid powder. The Al content was 14.0 wt%.
[0082] (2) In the reaction flask, add 120 mg of the above (1) white solid powder and 10.0 mg of the (L1)3Zr2Cl4 complex synthesized in Example 1, add 20 ml of toluene, and stir for 30 minutes.
[0083] (3) In a 2-liter stainless steel autoclave, after nitrogen blowing and ethylene replacement for many times, add 1 liter of hexane, the catalyst slurry obtained in (2) above and 2 mmoles of triethylaluminum, and feed Ethylene, and react at 1.0Mpa, 70°C for 2 hours. After cooling down, filter and dr...
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