Ligand based on pyridine structure and preparation method thereof, and supported catalyst based on pyridine structure and preparation method and application thereof

A technology of pyridine and ligands, which is applied in ethylene oligomerization, preparation, ligands based on pyridine structure and its preparation, and the field of supported catalysts based on pyridine structure, which can solve the problems of difficult equipment blockage and avoid equipment blockage , high target product selectivity, and the effect of reducing the probability of clogged pipelines

Active Publication Date: 2021-06-22
WANHUA CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the deficiencies in the prior art, the invention provides a ligand based on the pyridine structure and its preparation method, a supported catalyst based on the pyridine structure, its preparation method and its application in ethylene oligomerization. The supported catalyst prepared by the ligand will become the at

Method used

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  • Ligand based on pyridine structure and preparation method thereof, and supported catalyst based on pyridine structure and preparation method and application thereof
  • Ligand based on pyridine structure and preparation method thereof, and supported catalyst based on pyridine structure and preparation method and application thereof
  • Ligand based on pyridine structure and preparation method thereof, and supported catalyst based on pyridine structure and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0086] Example 1

[0087] The preparation method of ligand (L1):

[0088] 1) The 2,6-dibromo-4-methylpyridine (105.5 mmol) and aqueous methamide (211 mmol) were first heated at 180 ° C for 5 h, and then filtered, water (400 mL) and dichloromethane were added to the filtrate. 200 mL) EtOAc (EtOAc) EtOAc (EtOAc) EtOAc (EtOAc) The mixed solvent was allowed to give the product.

[0089] The product (80 mmol) was dissolved in acetonitrile (100 mL) solvent, then n-butyl lithium (160 mmol) was added at -80 ° C, and the reaction was added to -5 ° C, and the temperature was added to -5 ° C. 1H, the reaction liquid was purified by the column chromatography (a high diameter ratio of 2, the residence time was 2 min), and the mixed solvent of ethyl acetate and n-hexane of 1: 1 were dried, and the ligand L1 was obtained.

[0090]

[0091] The core magnetic data of the ligand (L1) is as follows: 1H NMR (400 MHz, CDCl3): 7.35 ~ 7.42 (m, 20H), 5.74 (S, 2H), 2.36 (S, 3H).

[0092] 2) At a nitroge...

Example Embodiment

[0095] Example 2

[0096] The kit (L2) is different from the preparation method in Example 1 in:

[0097]1) The 2,6-dibromo-4-methylpyridine (105.5 mmol) and isopropylamine (232.1 mmol) were first heated at 185 ° C for 6 h, and then filtered, water (600 ml) and dichloromethane were added to the filtrate. 200 mL) EtOAc (EtOAc) EtOAc (EtOAc) EtOAc (EtOAc) The mixed solvent was allowed to give the product.

[0098] The product was dissolved in acetonitrile (80 mmol) solvent, then n-butyl lithium (176 mmol) was added at -75 ° C, and the reaction was added to -3 ° C. After the temperature was added to -3 ° C, then the diphenylphosphine (176 mmol) was added, and the reaction was 2 h, the reaction The liquid was purified by the column chromatography (a high diameter ratio of 2, the residence time was 2 min) purified, and the mixed solvent of ethyl acetate and n-hexane of 1: 1 was dried, and the ligand L2 was obtained.

[0099]

[0100] The nuclear magnetic data of the above ligand (L2)...

Example Embodiment

[0104] Example 3

[0105] The preparation method of the ligand (L3) and the first embodiment is to:

[0106] 1) First, 2,6-dibromo-4-methylpyridine (105.5 mmol) and tert-butlamine (263.8 mmol) were heated at 190 ° C for 8 h, and then filtered, water (800 ml) and dichloromethane were added to the filtrate (200ml Extraction, vacuum conditions were removed to remove dichloromethane, and the resulting product was column chromatography (high diameter ratio of 2, the residence time was purified), and the magazine phase was 1: 1 of ethyl acetate and n-hexane. The mixed solvent was dried.

[0107] The product was dissolved in acetonitrile (80 mmol) solvent, then n-butyl lithium (192 mmol) was added at -70 ° C, and the reaction was added to 0 ° C, and the reaction was added to 0 ° C. The column chromatography (a high diameter ratio of 2, the residence time was 2 min) purified, the mixed solvent of ethyl acetate and n-hexane of 1: 1, and the ligand L3 was obtained after drying.

[0108]

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Abstract

The invention provides a ligand based on a pyridine structure and a preparation method thereof, and a supported catalyst based on the pyridine structure, a preparation method of the supported catalyst and application of the supported catalyst in ethylene oligomerization. A catalytic system comprises the ligand, a metal precursor with chromium as the center and silica gel. When the supported catalyst prepared from the ligand is used in ethylene oligomerization, the form of a polymer in ethylene oligomerization can be changed, so that the probability of blockage of a reaction kettle is greatly reduced, and continuous operation of a device is ensured.

Description

technical field [0001] The invention relates to the field of ethylene oligomerization catalysts, and relates to a ligand based on a pyridine structure and a preparation method thereof, a supported catalyst based on a pyridine structure, a preparation method and an application thereof in ethylene oligomerization. Background technique [0002] Linear α-olefin is an important commodity chemical intermediate, which can be used to produce plasticizers, additives, surfactants and lubricating oils, and more importantly, it can also be used to copolymerize with ethylene to form polymers. Linear α-olefins are important comonomers for the production of polymers with excellent properties and play an irreplaceable role in industrial production. For example, α-olefins are often added as comonomers in the industrial production of linear low-density polyethylene (LLDPE) and high-density polyethylene (HDPE), in which 1-hexene or 1-octene is copolymerized with ethylene to form a polymer It ...

Claims

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Application Information

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IPC IPC(8): C07F9/58B01J31/24C07C2/36C07C11/02
CPCC07F9/58B01J31/2409C07C2/36C07C2531/24B01J2531/62B01J2531/0213B01J2231/20C07C11/02Y02P20/52
Inventor 陈冠良张彦雨刘帮明郭华陈海波
Owner WANHUA CHEM GRP
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