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Supported bridged bis-phenoxy IVB metal catalyst and preparation method thereof
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A metal catalyst, bisphenoxy technology, applied in the field of supported bridged bisphenoxy IVB metal catalyst and its preparation, can solve the problem of low activity
Inactive Publication Date: 2016-06-08
SUN YAT SEN UNIV
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According to the characteristics of the [ONNO] type bridged bisphenoxy IVB metal catalyst skeleton ligand, the [ONNO] type bridged bisphenoxy IVB metal catalyst is supported on MgCl 2 / Et n Al(OR) 3-n A new type of supported catalyst is formed on the carrier to solve the problem of low activity of the homogeneous [ONNO] type bridged bisphenoxy IVB metal catalyst. At the same time, its kinetic reaction is stable and efficient, and it has high catalytic activity. It can be prepared branched polyethylene
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Embodiment 1
[0045] Example 1 Synthesis of Ligand Precursor L1
[0046] Add ethanol 100mL, 3,5-di-tert-butyl salicylaldehyde 11.7g, o-phenylenediamine 2.45g, N 2 Protected, heated to reflux for 6-8 hours, cooled to room temperature and precipitated a yellow precipitate, after suction filtration, dried at 50°C to obtain a yellow cotton flocculent solid, yield: 56.4%, to obtain diimine type [ONNO] type bridged bisphenoxy The metal catalyst ligand precursor is denoted as L1. 1 HNMR (300MHz, CDCl 3 ):δ:1.31(s,18H,C(CH 3 ) 3 ),1.42(s,18H,C(CH 3 ) 3 ),7.22(m,4H,Ar-H),7.30(m,2H,Ar-H),7.42(m,2H,Ar-H),8.63(s,2H,C=),13.48(s,2H ,OH).
Embodiment 2
[0047] Example 2 Synthesis of Ligand Precursor L2
[0048] Add 100mL of ethanol, 15.6g of 3,5-di-tert-butyl salicylaldehyde, 2.2mL of ethylenediamine into a 250mL round bottom flask equipped with a magnet, N 2 Protected, heated to reflux for 4-6 hours, cooled to room temperature and precipitated a yellow precipitate, filtered, and dried at 50°C to obtain a yellow cotton-like solid, yield: 89.4%, to obtain a diimine type [ONNO] type bridged bisphenoxide metal The catalyst ligand precursor is denoted as L2. 1 HNMR (300MHz, CDCl 3 ):δ:1.28(s,18H,C(CH 3 ) 3 ),1.43(s,18H,CH(CH 3 ) 3 ),7.04(d,J=2.4Hz,2H,Ar-H),7.34(J=2.4Hz,2H,Ar-H),8.36(s,2H,C=),13.59(s,2H,OH)
Embodiment 3
[0049] Example 3 Synthesis of [ONNO] type bridged bisphenoxy metal catalyst 1
[0050] At a temperature of -20 ° Under C, add 2.536g of ligand L1 to the Sehlenk bottle under nitrogenatmosphere, slowly add 5.0mL of 1.0mol / L titaniumtetrachloridetoluene solution dropwise, stir at this temperature for 60min, then rise to room temperature and continue stirring for 24h , remove the toluenesolvent by vacuum filtration; wash with n-hexane, filter, and remove the n-hexanesolvent by vacuum filtration to obtain 2.81g gray powder with a yield of 92%. Elemental analysis (C 36 h 46 Cl 2 N 2 o 2 Ti, mass %), theoretical value: C, 65.76; H, 7.05; N, 4.2.; measured value: C, 64.93; H, 6.97; N, 4.2.
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Abstract
The invention discloses a supported bridged bis-phenoxy IVB metal catalyst and a preparation method thereof. The structural formula of the active component [ONNO]MX2 of the catalyst is disclosed as Formula (I) or Formula (II). The active component of the catalyst is supported on a triethyl-aluminum-modified MgCl2 / EtnAl(OR)[3-n] supporter, wherein R is C2-C5 straight-chain alkyl; and n represents the quantity of hydroxyl hydrogens substituted by triethyl aluminum in ethanol, and n=0-3. According to the characteristics of the [ONNO] bridged bis-phenoxy IVB metal catalyst framework ligand, the [ONNO] bridged bis-phenoxy IVB metal catalyst is supported on the MgCl2 / EtnAl(OR)[3-n] supporter to form a novel supported catalyst, thereby solving the problem of low activity in the homogeneous [ONNO] bridged bis-phenoxy IVB metal catalyst. The kinetic reaction of the novel supported catalyst is stable and efficient, has higher catalytic activity, and can be used for preparing branched polyethylene.
Description
technical field [0001] The invention belongs to the field of catalytic polymerization of olefins, and in particular relates to a supported bridged bisphenoxy IVB metal catalyst and a preparation method thereof. Background technique [0002] Polyethylene is the most demanded general-purpose plastic in the world. It is characterized by low price and good performance. It can be widely used in industry, agriculture and daily life, and occupies a pivotal position in the plastics industry. Therefore, the research on ethylenepolymerization catalysts has always been an academic Research hotspots in the world and industry. Kol et al. (Tshuva, E.Y.; Goldberg, I.; Kol, M.J.Am.Chem.Soc., 2000, 122, 10706.) first discovered in 2000 that [ONNO] type bridging catalysts have certain activity for ethylenepolymerization. With further research, it is found that the homogeneous [ONNO] type bridged catalyst has the following disadvantages for ethylene polymerization due to its own structural ...
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