Imine compound activated iron polyolefin catalyzer

A technology of polyolefin catalysts and compounds, applied in the field of iron-based polyolefin catalysts

Inactive Publication Date: 2008-01-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] U.S. Patent US5955555 discloses that iron-based catalysts containing pyridinediimine can prepare linear polyethylene, and Chinese patent CN1431236 discloses a catalyst for preparing bimodal polyethylene, but bot

Method used

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  • Imine compound activated iron polyolefin catalyzer
  • Imine compound activated iron polyolefin catalyzer
  • Imine compound activated iron polyolefin catalyzer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation of embodiment 1 Schiff base

[0037]

[0038] With 30mL absolute ethanol as solvent, add 2,6-dimethylaniline (1.94g, 16.0mmol) and 2,6-diacetylpyridine (2.61g, 16.0mmol) successively, add dropwise 1mL formic acid as catalyst, room temperature Under stirring for 48h. A yellow precipitate appeared, filtered, washed with cold absolute ethanol three times, and recrystallized with hot ethanol to obtain 3.21 g of yellow needle-shaped Schiff base crystals, with a yield of 75.4%.

[0039] H NMR spectrum 1 H-NMR (400MHz, CDCl 3 , TMS): δ=2.02 (s, 6H, CH 3 ), 2.22(s,3H,C(NAr)CH 3 ), 2.76(s, 3H, C(O)CH3 ), 6.89-7.10(m, 3H Ar-H), 7.96(m, 1H, Py-H), 8.10(d, 1H, Py-H), 8.56(d, 1H, Py-H).

[0040] Elemental Analysis C 17 h 18 N 2 O (%): calcd. C 76.67, H 6.81, N 10.53; found C 76.45, H 6.54, N 10.41.

Embodiment 2

[0041] The preparation of embodiment 2 Schiff base

[0042]

[0043] 2,6-diisopropylaniline (2.83g, 16.0mmol) was used to replace 2,6-dimethylaniline, and other operations were the same as in Example 1 to obtain 4.25g of yellow needle-shaped Schiff base crystals, with a yield of 82.5% .

[0044] H NMR spectrum 1 H-NMRH NMR (400MHz, CDCl 3 , TMS): δ=1.16-1.17(m, 12H, CH(CH 3 ) 4 ), 2.28(s,3H,C(NAr)CH 3 ), 2.74(sept, 2H, CH(CH 3 ) 2 ), 2.81(s, 3H, C(O)CH 3 ), 7.08-7.22(m, 3H, Ar-H), 7.96(t, 1H, Py-H), 8.16(d, 1H, Py-H), 8.56(d, 1H, Py-H).

[0045] Elemental Analysis: C 21 h 26 N 2 O (%): calcd. C 78.22, H 8.13, N 8.69; found C 78.39, H 8.17, N 8.84.

Embodiment 3

[0046] Example 3 Preparation of bridged pyridinediimine compound

[0047] Using the Schiff base (1.5g, 5.63mmol) obtained in Example 1 and two (3,5-dimethyl-4-aminophenyl) methane (0.72g, 2.81mmol), p-toluenesulfonic acid as a catalyst ( 0.05g), heated and stirred, separated into water and refluxed for 15h, removed most of the solvent, cooled and precipitated a yellow precipitate, filtered, and washed with ethanol several times to obtain the bridged pyridinediimine compound L 1 1.75 g, yield 83.0%.

[0048] ESI-MS: m / z=751.5[M + ].

[0049] H NMR spectrum 1 HNMR (400MHz, DCCl 3 , TMS): δ=2.04(m, 24H, Ar-Me), 2.27(m, 12H, ArN=CMe), 3.88(s, 2H, -CH 2 -), 6.95-7.09(m, 10H, Ar-H), 7.92(t, 2H, Py-H p ), 8.50 (d, 4H, Py-H m ).

[0050] Elemental Analysis: C 51 h 54 N 6 (%): Calcd.C 81.56.H 7.25.N 11.19; Found: C81.48.H 7.19.N 11.25

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Abstract

The invention discloses an iron catalysts for polyolefine activated by the imine compounds, which comprises bridge-linked bis (imino) pyridyl compound in the structural formula (I) of the instruction book and FeAA or acetylacetone ferrous iron and MAO or alkyl aluminium compound. When carrying out the polymerization of the polyethylene, the high molecular weight polyethylene with molecular weight distribution from the singlet to the doublet can be gained by changing the polymerization condition. In the polyethylene with doublet distribution, the small molecular weight is obviously smaller than the occupied proportion of the large molecular weight, that is, the large molecular weight is dominant. The doublet molecular weight distribution can embody the good processability and can keep stronger mechanical property.

Description

technical field [0001] The invention relates to a polyolefin catalyst, in particular to an iron-based polyolefin catalyst activated by imine compounds. Background technique [0002] In 1998 Brookhart's article "Highly Active Iron and Cobalt Catalysts for the Polymeriza tion of Ethylene" ("J Am Chem Soc", 1998, 120(16): 4049-4050.), Gibson's article "Novel Olefin Polymerization Catalysts Based on Iron and Cobalt" ("Chem Commun", 1998, 7: 849-850.) reported novel pyridine diimide iron-based catalysts respectively, in methylalumoxane (MAO) or modified methylalumoxane (MMAO) Under the activation of ethylene, it can catalyze ethylene polymerization with high activity. When the amount of cocatalyst is increased to a certain extent, broad peak or even bimodal polyethylene can be obtained. Under normal pressure, the activity of this type of iron-based catalyst is not too high, and the molecular weight of the obtained polyethylene is also low. Although the molecular weight of polye...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/70
Inventor 孙俊权王临才
Owner ZHEJIANG UNIV
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