A kind of olefin polymerization catalyst and its preparation and application method

A technology of catalysts and main catalysts, applied in the direction of nickel organic compounds, etc., can solve the problems that late transition metal catalysts cannot meet the requirements

Active Publication Date: 2018-06-15
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 150-250°C. The original post-transition metal catalyst cannot meet the requirements of the existing gas phase and solution ethylene polymerization units

Method used

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  • A kind of olefin polymerization catalyst and its preparation and application method
  • A kind of olefin polymerization catalyst and its preparation and application method
  • A kind of olefin polymerization catalyst and its preparation and application method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The compound of this embodiment is shown in structural formula (II), wherein R 4 , R 8 is methyl, R 3 , R 7 , R 9 is hydrogen, X is Br.

[0062] 1) Preparation of ligand:

[0063] 11,12-(9,10-dihydro-9,10-ethyleneanthracene)bis(2-methylnaphthylamine):

[0064] 9,10-dihydro-9,10-ethylene anthracene-11,12-dione (1.14g, 4.8mmol) and 2-methylnaphthylamine (1.63g, 10.4mmol), 0.5g p-toluenesulfonic acid is The catalyst was refluxed in 100mL toluene for 1 day, and the solvent was removed after filtration, and the residue was dissolved in dichloromethane. The perbasic alumina column was washed with petroleum ether / ethyl acetate (20:1), and the product was separated and removed. The solvent gave a yellow solid in 46% yield. 1 H NMR (CDCl 3 , δ, ppm): 2.46 (s, 6H), 4.86 (s, 2H), 7.05-7.36 (m, 14H), 7.62-7.72 (m, 6H).

[0065] 2) Preparation of complex 1: [11,12-(9,10-dihydro-9,10-ethyleneanthracene) bis(2-methylnaphthylamine)]nickel(II) bromide: mix 10ml (DME)NiBr 2 (2...

Embodiment 2

[0068] 10atm ethylene polymerization: Dry the 1L stainless steel polymerization kettle equipped with mechanical stirring at 130°C for 6hrs continuously, vacuumize while it is hot and use N 2 Air replacement 3 times. 6.6 mg (10 μmol) of complex 1 were added and then evacuated and replaced with ethylene 3 times. 500 ml of hexane was injected, and 6.5 ml of methylaluminoxane (MMAO) (1.53 mol / l toluene solution) was added to make Al / Ni=1000. At 90°C, the ethylene pressure was maintained at 10 atm, and the reaction was vigorously stirred for 30 min. Neutralize with ethanol solution acidified with 5% hydrochloric acid to obtain polyethylene with a polymerization activity of 6.28×10 6 g·mol -1 (Ni)·h -1 .

Embodiment 3

[0070] The compound of this embodiment is shown in structural formula (II), wherein R 3 , R 4 , R 7 , R 8 is methyl, R 9 is hydrogen, X is Br.

[0071] 1) Preparation of ligand: 11,12-(9,10-dihydro-9,10-ethylene anthracene) bis(2,4-dimethylnaphthylamine): 9,10-dihydro-9, 10-ethylene anthracene-11,12-dione (1.82g, 7.8mmol) and 2,4-dimethylnaphthylamine (2.98g, 17.4mmol), 0.5g p-toluenesulfonic acid as catalyst, in 100mL toluene Reflux for 1 day, remove the solvent after filtration, dissolve the residue with dichloromethane, wash with petroleum ether / ethyl acetate (20:1) over a basic alumina column, separate the product, remove the solvent to obtain a yellow solid, and produce The rate is 42%. 1 H NMR (CDCl 3 , δ, ppm): 2.45 (s, 6H), 2.67 (s, 6H), 4.86 (s, 2H), 7.05-7.34 (m, 14H), 7.60-7.71 (m, 4H).

[0072] 2) Preparation of complex 2: [11,12-(9,10-dihydro-9,10-ethyleneanthracene) bis(2,4-dimethylnaphthylamine)]nickel(II) bromide : 10ml (DME)NiBr 2(155mg, 0.5mmol) dic...

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Abstract

The present invention relates to a kind of catalyst that is used for ethylene polymerization, and described catalyst comprises as the complex shown in (I) of chemical structure formula as main catalyst: in formula (1), X is halogen; R1-R8 can be same or different, each independently selected from a hydrogen atom, a halogen, a C1-C20 hydrocarbon group, a heterocyclic compound group or an organic group containing oxygen, nitrogen, boron, sulfur, phosphorus, silicon, germanium or tin atoms; and R1 and R2, R5 and R6 are optionally mutually ringed. The invention also provides a preparation method of the catalyst. The present invention also provides a method for olefin polymerization, which includes performing olefin polymerization reaction in the presence of the catalyst of the present invention.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a catalyst for olefin polymerization and a preparation method thereof. More specifically, it relates to a type of α-diimine nickel olefin polymerization catalyst and its preparation technology, and the application of the obtained catalyst in olefin polymerization. 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. In 2003, the world production of the materials used for key promotion in the industry reached 83.3 million tons; among them, polyethylene is the synthetic resin with the fastest development, the largest output and a wide range of uses, reaching 51.1 million tons that year. Industrialized polyethylene catalysts include...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/02C08F4/70C08F10/00C08F210/16C07F15/04
Inventor 高榕刘东兵周俊领李岩廖浩瀚傅捷
Owner CHINA PETROLEUM & CHEM CORP
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