Diimine metal complex and preparation method and application thereof

A technology of metal complexes and diimines, applied in nickel organic compounds, chemical instruments and methods, compounds containing elements of Group 8/9/10/18 of the periodic table, etc., can solve the problem that late transition metal catalysts cannot meet the requirements And other issues

Active Publication Date: 2021-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing ethylene gas phase polymerization process requires a polymerization temperature of above 85°C, and the ethylene solution polymerization process requires a polymerization temperature of 130-250°C. The original post-transition metal catalyst cannot meet the requirements of the existing gas phase and solution ethylene polymerization devices

Method used

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  • Diimine metal complex and preparation method and application thereof
  • Diimine metal complex and preparation method and application thereof
  • Diimine metal complex and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071]

[0072] Complex Ni 1 preparation of

[0073] Will contain 0.277g (0.9mmol) (DME) NiBr 2 The ethanol solution (10mL) was slowly added dropwise to the ligand L containing 0.175g (0.6mmol) 1 dichloromethane solution (10 mL), stirred at room temperature for 6 h, and added anhydrous ether to precipitate. Filtration left the filter cake, washed the filter cake with anhydrous ether, and obtained yellow powdery solid Ni after vacuum drying. 1 . Yield: 70.2%. Elemental analysis (C 44 h 58 Br 6 N 4 Ni 3 o 2 ): C, 39.72; H, 4.39; N, 4.21; Experimental values ​​(%): C, 39.38; H, 4.60; N, 3.96.

[0074] The 1L stainless steel polymerization kettle equipped with mechanical stirring was continuously dried at 130°C for 6hrs, vacuumized while hot and heated with N 2 Air replacement 3 times. Inject 500ml of hexane, then add 5.0ml methylaluminoxane (MAO) (1.53mol / l toluene solution), add 3.3mg (2.5μmol) complex Ni 1 . At 60°C, the ethylene pressure was maintained at 10 ...

Embodiment 2

[0076] The 1L stainless steel polymerization kettle equipped with mechanical stirring was continuously dried at 130°C for 6hrs, vacuumized while hot and heated with N 2 Air replacement 3 times. Inject 500ml of hexane, then add 5.0ml methylaluminoxane (MAO) (1.53mol / l toluene solution), add 3.3mg (2.5μmol) complex Ni 1 . At 80°C, the ethylene pressure was maintained at 10 atm, and the reaction was vigorously stirred for 30 min. Neutralized with ethanol solution acidified with 10 wt% hydrochloric acid to obtain polyethylene, the results are shown in Table 1.

Embodiment 3

[0078] The 1L stainless steel polymerization kettle equipped with mechanical stirring was continuously dried at 130°C for 6hrs, vacuumized while hot and heated with N 2 Air replacement 3 times. Inject 500ml of hexane, 10ml of 1-hexene, then add 5.0ml of methylaluminoxane (MAO) (1.53mol / l toluene solution), add 3.3mg (2.5μmol) of the complex Ni 1 . At 80°C, the ethylene pressure was maintained at 10 atm, and the reaction was vigorously stirred for 30 min. Neutralized with ethanol solution acidified with 10 wt% hydrochloric acid to obtain polyethylene, the results are shown in Table 1.

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Abstract

The invention relates to a diimine metal complex as shown in a formula I and a preparation method and application thereof, and the diimine metal complex is used as a main catalyst of a catalyst for olefin polymerization and can catalyze ethylene polymerization at a relatively high temperature to prepare high-molecular-weight branched polyethylene.

Description

technical field [0001] The invention relates to a diimine metal complex and its preparation method and application. Background technique [0002] my country is the country with the fastest growing consumption of synthetic resin and the largest importer of synthetic resin. At present, the proportion of polyolefin production is nearly 60%. Compared with other resin materials, olefin resin has excellent environmental coordination. It is estimated that the apparent consumption of polyolefins in my country will be 67.77 million tons in 2019, and the consumption of polyethylene will reach 34.59 million tons. Industrialized polyethylene catalysts have Ziegler-Natta type catalysts (DE Pat 889229 (1953); IT Pat 545332 (1956) and IT Pat 536899 (1955); Chem. Rev., 2000, 100, 1169 and related documents in this special edition), Phillips type catalyst (Belg.Pat.530617 (1955); Chem.Rev.1996,96,3327) and metallocene type catalyst (W.Kaminsky, Metalorganic Catalysts for Synthesis and Polyme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04C08F110/02C08F210/02C08F220/64C08F216/04C08F4/70
CPCC07F15/045C08F110/02C08F210/02C08F2410/03C08F216/04C08F220/64C08F4/7006
Inventor 高榕郭子芳赖菁菁李昕阳刘东兵顾元宁李岩傅捷
Owner CHINA PETROLEUM & CHEM CORP
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