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

A technology of olefin polymerization and catalyst, which is applied in the direction of nickel organic compounds, etc., can solve the problems that late transition metal catalysts cannot meet the requirements, and achieve the effect of simple and easy ligand synthesis method, high copolymerization activity and high polymerization activity

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 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 devices

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

[0054] The compound of this embodiment is shown in structural formula (I), wherein R 1 , R 3 , R 4 and R 6 is methyl, R 2 and R 5 is hydrogen, X is Br.

[0055] 1) Preparation of ligand:

[0056] 11,12-(9,10-dihydro-9,10-ethyleneanthracene)bis(2,6-dimethylaniline):

[0057] 9,10-dihydro-9,10-ethylene anthracene-11,12-dione (1.14g, 4.8mmol) and 2,6-methylaniline (1.3ml, 10.4mmol), 2ml acetic acid as catalyst, in Reflux in 100mL ethanol for 1 day, remove the solvent after filtration, dissolve the residue with dichloromethane, rinse with petroleum ether / ethyl acetate (20:1) on a perbasic alumina column, isolate the product, remove the solvent to obtain a yellow Solid 1.97g, yield 92%. 1 HNMR (CDCl 3 ,δ,ppm): 1.88(s,12H), 4.85(s,2H), 7.05-7.24(m,14H). Elemental analysis (C 32 h 28 N 2 ) Theoretical value (%): C, 87.36; H, 6.54; N, 6.27; Experimental value (%): C, 87.24; H, 6.41; N, 6.36.

[0058] 2) Preparation of complex 1:

[0059] Preparation of [11,12-(9,10-dihy...

Embodiment 2

[0063] 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. Add 6.6 mg (10 μmol) of complex 1 prepared in Example 1 and then evacuate and replace with ethylene three 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 1.25×10 6 g·mol -1 (Ni)·h -1 , and the results are shown in Table 1.

Embodiment 3

[0065] The compound of this embodiment is shown in structural formula (I), wherein R 1 , R 3 , R 4 and R 6 is ethyl, R 2 and R 5 is hydrogen, X is Br.

[0066] 1) Preparation of ligand:

[0067] 11,12-(9,10-dihydro-9,10-ethyleneanthracene) bis(2,6-diethylaniline): 9,10-dihydro-9,10-ethyleneanthracene-11, 12-diketone (1.82g, 7.8mmol) and 2,6-diethylaniline (3.0ml, 17.4mmol), 2ml of acetic acid as a catalyst, refluxed in 100mL of ethanol for 1 day, removed the solvent after filtration, and the residue was washed with di Methane chloride was dissolved, and the column of perbasic alumina was rinsed with petroleum ether / ethyl acetate (20:1) to isolate the product, and the solvent was removed to obtain 1.97 g of a yellow solid, with a yield of 91%. 1 HNMR (CDCl 3 , δ, ppm): 1.06 (t, 12H, J = 7.5Hz), 2.18 (dd, 8H, J = 7.5Hz), 4.86 (s, 2H), 7.15-7.20 (m, 14H). Elemental analysis (C 36 h 36 N 2 ) Theoretical value (%): C, 87.05; H, 7.31; N, 5.64; Experimental value (%): C, ...

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PUM

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Abstract

The invention provides an olefin polymerization catalyst. The invention is characterized in that the catalyst comprises a complex whose chemical structural formula is shown as Formula (I) as the main catalyst, wherein the values of the R1-R6 can be identical or different; and the R1-R6 are respectively and independently selected from alkyl or halogen, wherein the X stands for halogen. The invention further provides a preparation method of the olefin polymerization catalyst. 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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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F4/70C07F15/04
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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