Olefin polymerization catalyst as well as preparation method and application method thereof

A catalyst and ethylene polymerization technology, 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: 2016-04-13
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 polym...

Method used

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  • Olefin polymerization catalyst as well as preparation method and application method thereof
  • Olefin polymerization catalyst as well as preparation method and application method thereof
  • Olefin polymerization catalyst as well as preparation method and application method thereof

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 HNMR (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 (27...

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 HNMR (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) dich...

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Abstract

The invention relates to a catalyst for olefin polymerization. The catalyst comprises a complex whose chemical structural formula is shown as Formula (I) as the main catalyst. In the Formula (I), the X stands for halogen; the values of the R1-R8 can be identical or different; the R1-R8 are respectively and independently selected from hydrogen atom, halogen, C1-C20 alkyls, heterocyclic compound group or organic groups containing oxygen atom, nitrogen atom, boron atom, sulfur atom, phosphorus atom, silicon atom, germanium atom or tin atom; and loops are optionally formed by the R1 and the R2 as well as the R5 and the R6 mutually. And the invention also provides an olefin polymerization method, wherein the olefin polymerization method comprises the step of carrying on olefin polymerization reaction under the existence of the olefin polymerization catalyst provided by the 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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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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