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Nickel catalyst with high steric hindrance, synthesis method therefor and application of nickel catalyst

A technology of nickel catalyst and synthesis method, applied in nickel organic compounds, chemical instruments and methods, compounds containing elements of Group 8/9/10/18 of the periodic table, etc. Limitation, insufficient catalyst activity, etc., to achieve the effect of increasing instability, high regularity, and reducing the rate of transfer

Pending Publication Date: 2019-12-13
NINGXIA VOCATIONAL TECHN COLLEGE OF IND & COMMERCE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing late-transition metal catalysts cannot effectively increase the degree of branching of the polymerization product and control the stereoregularity of the polymerization product due to insufficient catalyst activity when catalyzing the polymerization. many restrictions

Method used

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  • Nickel catalyst with high steric hindrance, synthesis method therefor and application of nickel catalyst
  • Nickel catalyst with high steric hindrance, synthesis method therefor and application of nickel catalyst
  • Nickel catalyst with high steric hindrance, synthesis method therefor and application of nickel catalyst

Examples

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Embodiment 1

[0023] A structure is a large steric hindered nickel catalyst of α-diimine nickel (II) substituted by an ortho-phenyl vinyl group, and its synthesis method is as follows:

[0024] (1) Synthesis of 2,3-dimethyl-6-phenylvinylaniline: 2,3-dimethylaniline (0.24g, 2.00mmol), styrene (0.52g, 5.00mmol), xylene (2mL), trifluoromethanesulfonic acid (0.06g, 0.4mmol) were sequentially added to a 100mL Schlenk bottle, reacted at 260°C for 48h, and the residue obtained was washed three times with ether (3×10mL) to remove volatile substances , and then separated by column chromatography with petroleum ether / ethyl acetate (volume / volume=30:1), to obtain 0.28 g (62% yield) of a light yellow liquid whose structure is 2,3-dimethyl-6 -Phenylvinylaniline. The specific reaction principle is as follows.

[0025]

[0026] (2) Synthesis of ligands: 2,3-dimethyl-6-phenylvinylaniline (0.49g, 2.2mmol) and diacetyl (0.087g, 1.00mmol) were added to a 100mL round bottom flask, Then add 40mL of absolu...

Embodiment 2

[0033] Materials and reagents in Example 1: All organometallic reactions were carried out under N 2 Carry out under protection; Solvent all needs to dry deoxygenation treatment; O-dichlorobenzene (analytical pure) and dichloromethane, use Molecular sieve pre-dried and then in N 2 CaH 2 Reflux, evaporate before use; high-purity N 2 and polymer grade ethylene monomer, deoxygenated and dried before use; toluene, ether (analytical pure), after molecular sieve dehydration, added metal sodium to reflux under nitrogen protection, and steamed before use; anhydrous methanol, ethanol, chloroform ( Analytical pure), used directly; DME (1,2-dimethoxyethane) (analytical pure), used Molecular sieve drying; 2,3-dimethylaniline, styrene and trifluoromethanesulfonic acid are all products of Aladdin Company, and diethylaluminum chloride (0.9M toluene solution) is a product of Aldrich Company.

Embodiment 3

[0035] A large sterically hindered nickel catalyst with a structure of α-diimine nickel (II) substituted by an ortho-phenylvinyl group is used as a late transition metal catalyst for the polymerization of ethylene. The specific polymerization process is as follows.

[0036] The 250mL Schlenk polymerization bottle with a magnetic stirring bar was subjected to vacuum-nitrogen cycle replacement three times. Under a nitrogen atmosphere, 50mL of toluene dehydrated and deoxygenated by metal sodium reflux was injected with a syringe, and then ethylene was introduced to fully absorb ethylene until it was saturated. Add 3.5mL (0.9M) cocatalyst DEAC (diethylaluminum chloride) into the reaction flask with a syringe, stir at 60°C for 15 minutes, and then use a syringe to dissolve 5mmol of 1 nickel catalyst, maintain the pressure required for ethylene polymerization (0.2bar), and continue to polymerize at 60°C for 10 minutes; then use 100mL of 5% to 95% hydrochloric acid-methanol solution t...

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Abstract

The invention belongs to the technical field of chemical synthesis and relates to a nickel catalyst with high steric hindrance, a synthesis method therefor and an application of the nickel catalyst. The nickel catalyst with high steric hindrance structurally is an ortho phenyl vinyl substituted alpha-diimine nickel (II) catalyst and can be applied to an ethylene and styrene polymerization processas a late-transition metal catalyst. According to the nickel catalyst with high steric hindrance, through introducing a group with high steric hindrance, the electron cloud density of a metal center of the catalyst is effectively protected, the activity of the catalyst is improved, and polyethylene can have a relatively high degree of branching; and meanwhile, monomers can better have stereoselective insertion, and thus, isotactic polystyrene with syndiotactic height is obtained.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a large steric hindrance nickel catalyst and its synthesis method and application. Background technique [0002] In real life, polyethylene and polystyrene products have become indispensable commercial products and have a very wide range of applications, such as various films, food packaging, wires and cables, high-performance fibers and medical supplies. At the same time, since the discovery of α-diimine nickel catalyst by Brookhart et al., there has been great interest in the design of homogeneous nickel-based polymerization, that is, by designing different reaction conditions, high activity, high molecular weight Polyethylene, or linear, hyperbranched polymer topology, or polystyrene with controlled stereoregularity, etc. However, the existing late-transition metal catalysts cannot effectively increase the degree of branching of the polymerization product and control...

Claims

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Application Information

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IPC IPC(8): C08F4/70C08F110/02C08F112/08C07F15/04
CPCC07F15/045C08F110/02C08F112/08C08F4/7006
Inventor 赵杰薛新巧
Owner NINGXIA VOCATIONAL TECHN COLLEGE OF IND & COMMERCE
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