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Bridged diamidino group-IV metal catalyst and method for preparing same

A metal catalyst and a bridging technology, which are applied in the field of bridged bisamidine group IV metal catalysts and their preparation, can solve the problems of complex synthesis methods, harsh synthesis conditions, easy deactivation and the like, and achieve simple preparation methods and easy-to-obtain raw materials. , the effect of low price

Inactive Publication Date: 2010-08-11
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, they all have defects such as harsh synthesis conditions and low total catalyst yield. In addition, the storage conditions of the catalyst are also very harsh, easy to deactivate, and the synthesis method is complicated, and the raw materials are not suitable for preparation. Therefore, new non-metallocene catalysts has become a research hotspot in recent years

Method used

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  • Bridged diamidino group-IV metal catalyst and method for preparing same
  • Bridged diamidino group-IV metal catalyst and method for preparing same
  • Bridged diamidino group-IV metal catalyst and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] (1) Preparation and characterization of ligand lithium salt

[0060] Under the protection of nitrogen and ice water bath, dimethylsilyl bridged diphenylamine (6.0g, 24.8mmol) was dissolved in ether (200cm 3 ), under stirring, slowly add LiBu n n-hexane solution (2.8mol dm -3 , 17.7cm 3 , 49.6mmol), after the reaction mixture returned to room temperature, continued to stir for 2 hours, cooled the reaction solution to 0°C, and added PhCN (5.06cm 3 , 49.6mmol), after the reaction mixture returned to room temperature, continue to stir for 5 hours, and recrystallize the white solid obtained after the reaction with tetrahydrofuran to obtain a yellow crystal bridged bis-amidine ligand lithium salt 1a, Yield: 17.2g (93%), mp 86-88°C. 1 H NMR (300MHz, C 6 D. 6 ): δ7.46-6.67 (m, 20H; phenyls), 3.52 (t, J HH =6.0Hz, 16H; OCH 2 of THF), 1.35 (p, J HH =3.3, 2.7Hz, 16H; 3, 4-2CH 2 of THF), 0.24 (s, 3H; SiMe 2 ); 13 CNMR (75MHz, C 6 D. 6 ): δ175.7 (N-C-N), 154.0, 143.8...

Embodiment 2

[0068] Preparation and characterization of catalyst 3b

[0069] (1) The preparation of ligand lithium salt is the same as in Example 1.

[0070] (2) Vacuumize the Schlenk bottle and pass N 2 After replacing three times, add 1b (1.43g, 2.42mmol) and 20mL of tetrahydrofuran, and slowly add ZrCl 4 (0.56g, 2.42mmol), the reaction mixture was gradually returned to room temperature, and stirring was continued for 12 hours. The reaction solvent and volatile matter were drained under vacuum, and the residue was dissolved in dichloromethane (25 mL), extracted and filtered, concentrated under reduced pressure, and left for a period of time to grow pale yellow crystal compound 3b. Yield: 1.02g (63%).M.p.: 227~229℃. 1 H NMR (300MHz, CDCl 3 ): δ7.33~6.83(m, 16H; phenyls), 3.75(s, 4H; OCH 2 of THF), 2.30(s, 12H; Me on phenyls), 1.54(s, 4H; 3,4-2CH 2 of THF), 0.68 (s, 6H; SiMe 2 ); 13 C NMR (75MHz, CDCl 3 ): δ176.6 (N-C-N), 147.0, 137.7, 135.4, 133.3, 131.3, 130.6, 130.1, 126.7 (p...

Embodiment 3

[0072] Preparation and characterization of catalyst 3c

[0073] (1) The preparation of ligand lithium salt is the same as in Example 1.

[0074] (2) Vacuumize the Schlenk bottle and pass N 2 After replacing three times, add 1c (1.31g, 0.85mmol) and 20mL of tetrahydrofuran, and slowly add ZrCl 4 (0.40g, 1.70mmol), the reaction mixture was gradually returned to room temperature, and stirring was continued for 12 hours. The reaction solvent and volatile matter were drained under vacuum, and the residue was dissolved in dichloromethane (25 mL), extracted and filtered, concentrated under reduced pressure, and a colorless crystal compound 3c was grown after standing for a period of time. Yield: 0.95g (66%).M.p.: 256~257℃. 1 H NMR (300MHz, CDCl 3 ): δ7.30~7.00(m, 16H; phenyls), 3.82(t, 4H; OCH 2 of THF), 3.66 (m, 4H; CH (CH 3 ) 2 ), 1.58 (p, 4H; 3, 4-2CH 2 of THF), 1.08, 0.70(d, s, 24H; CH(CH 3 ) 2 ), 0.75(s, 6H; SiMe 2 ); 13 C NMR (75MHz, CDCl 3 ): δ175.0 (N-C-N), 146...

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Abstract

The invention provides a bridged diamidino group-IV metal catalyst, which relates to an olefin polymerization catalyst, in particular to a compound taking metals of a group IV as central atoms and a seven-element skeleton with an N-C-N-Si-N-C-N characteristic as a ligand. A method for preparing the bridged diamidino group-IV metal catalyst comprises the following steps: in the protection of nitrogen, taking bridging diamine as an initial raw material and converting the bridging diamine into a dilithium salt by utilizing butyl lithium; adding cyanophenyl into the dilithium salt to produce an addition reaction, forming a bridged diamidino ligand after migrating a silicon base twice, and performing a complex reaction on the polydentate ligand and group-IV metal chloride of the group IV to prepare bridged diamidino group-IV metal chloride; and reacting lithium methide with the bridged diamidino group-IV metal chloride to displace helium atoms to produce a methyl substitute. The synthesis method has the advantages of universal applicability, moderate reaction condition, simple and easily-obtained materials, low cost, simple steps and relatively higher productivity. The compound has good catalytic effect on the polyreaction of olefin.

Description

technical field [0001] The invention relates to a group IV transition metal catalyst for ethylene polymerization, in particular to a bridging bis-amidino group IV metal catalyst with an N-C-N-Si-N-C-N skeleton, a preparation method and application thereof. Background technique [0002] At present, industrialized olefin polymerization catalysts include Ziegler-Natta catalysts, Phillips catalysts and metallocene catalysts, etc. These catalysts can control the catalytic activity and polymer properties by adjusting the structure of the ligand. Brintzinger reported that a class of bridged metallocene catalysts not only has high activity, but also can control the stereo configuration of polymers (H. Schnutenhaus, H.H. Brintzinger, Angew. Chem, Int. Ed., 1979, 18, 777.). However, they all have defects such as harsh synthesis conditions and low total catalyst yield. In addition, the storage conditions of the catalyst are also very harsh, easy to deactivate, and the synthesis method ...

Claims

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Application Information

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IPC IPC(8): C08F4/64C08F4/659C08F10/00C08F10/02
Inventor 白生弟袁世芳刘滇生童红波
Owner SHANXI UNIV
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