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Ethylene oligomerization catalyst and preparation method and application thereof

A technology of ethylene oligomerization and catalyst, which is applied in the direction of catalysts, catalytic reactions, carbon compound catalysts, etc., can solve the problems of wide product distribution, easy blockage of pipelines, and high production costs, and achieve low polymer production, reduced dosage, and improved durability. The effect of thermal performance

Active Publication Date: 2020-10-30
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Homogeneous ethylene oligomerization catalysts generally need to carry out ethylene oligomerization reaction at low temperature (40-60°C), the precipitation of high polymers is easy to block the pipeline, the product distribution is wide, the separation is difficult, the energy consumption is large, and the production cost is high

Method used

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  • Ethylene oligomerization catalyst and preparation method and application thereof
  • Ethylene oligomerization catalyst and preparation method and application thereof
  • Ethylene oligomerization catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of Ligand I: Weigh quantitative 1mol of pyrrole and 1mol of 2-pyrrole acetaldehyde, add to 150ml of pentane solution, slowly add 0.2mol of phosphorus oxychloride, react for 3 to 5 hours and filter to obtain insoluble pentane solution The dipyrrole cation salt, the ionic salt is dissolved in the pentane solution of the calcium hydroxide suspension, and shaken vigorously for 3-15 minutes to obtain the pentane solution of the dipyrromethene. At -78°C, add an excess of 3 mol n-butyl lithium dropwise to the dipyrromethene pentane solution, slowly warm up to room temperature, stir for 3 to 6 hours, filter and slowly add 2.5 mol n-butyl lithium dropwise to the solution at -75°C Chlorophenylphosphine, stirred for 3-5 hours, stirred overnight at room temperature, purified by neutral alumina column chromatography, and recrystallized twice to obtain the ligand I product. The Ligand I structure is shown below:

[0036]

[0037] Ligand grafting on silica gel: All opera...

Embodiment 2

[0042] Preparation of ligand: same as Example 1.

[0043] Ligand grafting on silica gel: Same as Example 1.

[0044] Loading active component Cr: Same as Example 1.

[0045] Ethylene oligomerization: Heat a 500ml reactor to 120°C, vacuumize for 4 hours, replace nitrogen three times during this period, then vacuumize and fill hydrogen twice, wait for the temperature to cool to room temperature, add 200ml of refined methylcyclohexane, 1.0 ml MAO (10wt% toluene solution), turn on the stirrer, after the temperature is constant at 80°C, add 0.4g catalyst, pass in hydrogen at 0.5Mpa, pass in ethylene to 4.5MPa for oligomerization reaction, after 30min of reaction, turn off the ethylene The inlet valve is used to quickly cool down with a low-temperature circulating water bath, slowly release the pressure, and unload the kettle to obtain ethylene oligomerization products.

Embodiment 3

[0047] Preparation of ligand: same as Example 1.

[0048] Ligand grafting on silica gel: Same as Example 1.

[0049] Loading active component Cr: Same as Example 1.

[0050] Ethylene oligomerization: Heat a 500ml reactor to 120°C, vacuumize for 4 hours, replace nitrogen three times during this period, then vacuumize and fill hydrogen twice, wait for the temperature to cool to room temperature, add 200ml of refined methylcyclohexane, 1.34 ml MAO (10wt% toluene solution), turn on the stirrer, after the temperature is constant at 80°C, add 0.4g catalyst, pass in hydrogen at 0.5Mpa, pass in ethylene to 4.5MPa for oligomerization reaction, after 30min of reaction, turn off the ethylene The inlet valve is used to quickly cool down with a low-temperature circulating water bath, slowly release the pressure, and unload the kettle to obtain ethylene oligomerization products.

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Abstract

The present invention relates to an ethylene oligomerization catalyst and a preparation method and application thereof, the structure of the catalyst is shown in the specification, or R1 is selected from-CH2-,-(CH2) 2-,-(CH2) 3-,-(CH2) 4-,-C (CH3) 2-,-C (CH3) 2CH2-, a cyclohexyl linking group or a phenyl linking group, and R2 and R3 are respectively selected from chlorine or methyl. The preparation method of the catalyst comprises the following steps: (1) grafting a ligand on silica gel; and (2) loading an active component Cr. The catalyst disclosed by the invention and an aluminum alkyl cocatalyst form an ethylene oligomerization catalyst system; the catalyst can catalyze an ethylene oligomerization reaction with high activity, the catalytic activity of the carrier catalyst can reach 4.99* 10 < 6 > g product / (mol.Cr.h), the selectivity of 1-hexene and 1-octene with high added values is high, and the catalyst is easy to separate from the product.

Description

technical field [0001] The invention belongs to the field of ethylene oligomerization catalysis, and relates to an ethylene oligomerization catalyst, its preparation method and application. Background technique [0002] Linear α-olefins are an important class of organic chemical raw materials and are widely used in polyethylene comonomers, surfactants, lubricating oils and oil additives. With the development of the chemical industry, the demand for α-olefins continues to grow, and the demand for 1-hexene and 1-octene grows most rapidly. 1-Hexene is mainly used in the production of linear low-density polyethylene (LLDPE) and high-density polyethylene (HDPE), 1-octene, as an important organic raw material and chemical intermediate, is mainly used in the production of high-end polyethylene, polyolefin elastic Polymer (POE) and used as a raw material for the production of plasticizers, detergent alcohols and lubricating oil additives. At present, most of the linear α-olefin pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/24C07C2/36C07C11/107C07C11/02
CPCC07C2/36B01J31/2409C07C2531/24B01J2531/62B01J2231/20C07C11/107C07C11/02Y02P20/52
Inventor 刘帮明陈冠良马鹏杰黄玲燕张田财林小杰张彦雨
Owner WANHUA CHEM GRP CO LTD
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