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Transition metal catalyst for oligomerization and polymerization of ethylene and its prepn process and use

A catalyst and complex technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as limiting the development of ethylene oligomerization and polymerization industry

Active Publication Date: 2007-08-22
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, most of the above-mentioned catalysts are protected or covered by foreign patents, which seriously limits the development of my country's ethylene oligomerization and polymerization industry. It is imminent to research and develop ethylene oligomerization and polymerization catalysts with independent intellectual property rights.

Method used

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  • Transition metal catalyst for oligomerization and polymerization of ethylene and its prepn process and use
  • Transition metal catalyst for oligomerization and polymerization of ethylene and its prepn process and use
  • Transition metal catalyst for oligomerization and polymerization of ethylene and its prepn process and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] 1. The preparation of catalyst C1: Chromium chloride tetrahydrofuran (0.1315g, 0.35mmol) and corresponding benzimidazolpyridine L1 (0.1093g, 0.35mmol) are added in the Schlenk bottle, and the logical N 2 After three replacements, add treated dichloromethane (10ml), stir at room temperature for 24 hours, add anhydrous diethyl ether after concentration, and a green precipitate precipitates out. After filtering, vacuum-dry to obtain the complex 0.118g, C1 yield: 75.0 %. Elemental Analysis Theoretical Value C 19 h 12 C l3 CrN 5 : C, 48.59; H, 2.79; N, 14.91; Found: C, 48.30; H, 2.80; N, 14.54%. IR(KBr:cm -1 ): 3070 (v N-H ), 1609 (v C＝C ), 1468(δ N-H ), 1321, 1147, 998, 826, 754 (δ N-H ).

[0069] 2. Ethylene oligomerization: Dry the 250ml polymerization bottle equipped with a magnetic stirrer at 130°C for 6 hours continuously, vacuumize while it is hot and use N 2 Air replacement 3 times. Catalyst C1 (2.3 mg, 5 μmol) was added, followed by evacuation and replac...

Embodiment 2

[0071] 1. The preparation of catalyst C1 is the same as in Example 1.

[0072] 2. Ethylene oligomerization: Vacuumize a 250 ml stainless steel kettle equipped with a mechanical stirrer and a thermocouple, replace it with nitrogen for 3 times, and then replace it with ethylene for 2 times. After cooling to 40°C, sequentially add the toluene solution of catalyst C1 (0.9mg, 2μmol) and a certain amount of toluene, and finally add a certain amount of methylaluminoxane (1.46mol / L, 3.4ml) to make Al / Cr=1000 , the total volume of toluene is 100ml. The ethylene pressure was immediately raised to 10 atm and stirred vigorously at 40°C for 60 minutes. After cooling, take out a little reaction solution, neutralize the MAO in it with dilute hydrochloric acid at 0°C, take a small amount of toluene layer, dry it with anhydrous sodium sulfate, and measure the content and distribution of oligomers by gas chromatography. Oligomerization activity: 14.0×10 6 g(oligomer)·mol -1 (Cr) h -1 . Ol...

Embodiment 3

[0074] 1. The preparation of catalyst C1 is the same as in Example 1.

[0075] 2. Ethylene polymerization: Dry the 250ml polymerization bottle equipped with a magnetic stirrer at 130°C for 6 hours continuously, vacuumize it while it is hot and use N 2 Air replacement 3 times. Catalyst C1 (2.3 mg, 5 μmol) was added, followed by evacuation and replacement with ethylene twice. A certain amount of toluene (29.6ml) was injected with a syringe, and a hexane solution of diethylaluminum chloride (0.375ml) was added. Make Al / Cr = 150, keep the ethylene pressure of 1 atm at 25°C, and stir vigorously for 60 minutes. Add 5% hydrochloric acid ethanol solution to the reaction solution for neutralization, and a white solid precipitates out. After filtration it was vacuum dried for 12 hours. Obtained product 0.075g, polymerization activity: 1.5×10 4 g·mol -1 (Cr) h -1 .

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Abstract

The present invention discloses serial 2, 6-bisbenzimidazole pyridyl chromium halide complexes in the structure as shown. The present invention also discloses the preparation process of these novel complexes, composite catalyst including these novel complexes and their application in oligomerization and polymerization of ethylene. The complexes of the present invention are prepared with simple cheap materials, and have great modification space and high activity for oligomerization and polymerization of ethylene.

Description

Technical field: [0001] The invention relates to a transition metal catalyst for ethylene oligomerization and polymerization, in particular to a novel N-N-N tridentate ligand chromium complex catalyst and a preparation method thereof. The present invention also relates to a catalyst composition comprising the novel N-N-N tridentate ligand chromium complex catalyst and its use for catalyzing ethylene oligomerization and polymerization. Background technique: [0002] As we all know, there are currently two industrialized ethylene polymerization catalyst systems, one is the Ziegler-Natta catalyst, which is a binary system composed of transition metal salts and alkyl metal compounds, and the other is the chromium-based ethylene polymerization catalyst developed by Philips. . According to statistics, 1 / 3 of the world's total ethylene products are produced using chromium-based ethylene polymerization catalysts developed by Philips. Chromium-based catalysts have become the main c...

Claims

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Application Information

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IPC IPC(8): C07F11/00B01J31/22B01J31/12C07C2/26C07C2/34C08F10/02C08F4/60
CPCY02P20/52
Inventor 栗同林孙文华徐珂张文娟张树介素云
Owner CHINA PETROLEUM & CHEM CORP
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