Carbon nickel series olefin polymerization catalyst containing sulfur family elements as well as preparation and uses thereof
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A technology of olefin polymerization and chalcogen elements, which is applied in the field of nickel-based olefin polymerization catalysts and its preparation, can solve the problems of air sensitivity, intolerance, and low catalytic activity of catalysts
Inactive Publication Date: 2008-09-03
FUDAN UNIV
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[0003] The early transition metal titanium series catalysts have low catalytic activity, are sensitive to air, and cannot tolerate heteroatom monomers; the catalytic system composed of z
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Embodiment 1
[0022] Embodiment 1: Preparation of ligand L1:
[0023] Under the protection of high-purity argon, 0.01mol 1,1-bis(1-methylimidazolium)methane bromide salt, 0.01mol potassium carbonate, 0.02mol sulfur powder (the ratio of the amount of the three substances is 1:1: 2), 60mL of methanol or toluene or tetrahydrofuran is placed in a 100ml reaction flask, refluxed for 24 hours, cooled to room temperature, removed solvent, CH 2 Cl 2 or CHCl 3 After washing and filtering, the solvent was removed to obtain 1.63 g of colorless solid powder with a yield of 68%.
Embodiment 2
[0024] Embodiment 2: the preparation of ligand L2:
[0025] Under the protection of high-purity argon, with 0.01mol 1,1-bis(1-methylimidazolium) methane bromide salt, 0.01mol potassium carbonate, 0.02mol selenium powder (the ratio of the amount of the three substances is 1:1: 2), 60mL of methanol or toluene or tetrahydrofuran is placed in a 100ml reaction flask, refluxed for 24 hours, cooled to room temperature, removed solvent, CH 2 Cl 2 or CHCl 3 After washing and filtering, the solvent was removed to obtain 1.90 g of a colorless solid powder with a yield of 56%.
Embodiment 3
[0026] Embodiment 3: Preparation of ligand L3:
[0027] Under the protection of high-purity argon, 0.01mol 1,1-two (1-methylimidazolium) ethane bromide bromide, 0.01mol potassium carbonate, 0.02mol sulfur powder (the ratio of the amount of the three substances is 1:1 : 2), 60mL of methanol or toluene or tetrahydrofuran was placed in a 100ml reaction flask, refluxed for 24 hours, cooled to room temperature, solvent removed, CH 2 Cl 2 or CHCl 3 After washing and filtering, the solvent was removed to obtain 1.61 g of a colorless solid powder with a yield of 63%.
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Abstract
The invention belongs to an olefinic polymerization catalyst technical field, especially an olefinic polymerization catalyst of carbene nickel series containing sulfur family element and preparation method thereof and application. The catalyst is represented by formular: [L-NiBr2], wherein L represents double teeth ligand containing substituent sulfur or selenium carbene type which can coordinate with metal. Dibromomethane or dibromoethane and substituent imidazole are used as start material, and the double teeth ligand containing substituent sulfur or selenium carbene type is obtained after a series of reaction steps/ The ligand is respectively reacted with di(triphenyl phosphor) nickel dibromide of one molar mass, and then subjected to filtering, cleaning, and vacuum pumping and drying to finally obtain the corresponding nickel catalyst. The catalyst is coordinated with co-catalyst MAO or MMAO and used for catalysing the addition polymerization of norborene, with high catalytic activity. The invention has features of simplicity, good stability. The obtained polynorbornene product has high molecule weight, high glass-transition temperature and fine solubleness.
Description
technical field [0001] The invention belongs to the technical field of olefin polymerization catalysts, and in particular relates to a nickel-based olefin polymerization catalyst and its preparation method and application. technical background [0002] As the pillar industry of modern polymer materials, the development of polyolefin industry is an important symbol to measure the development of a country's petrochemical industry. Polyolefin products have greatly promoted the development of human civilization, and olefin polymerization catalysts are the key to the development of polyolefin industry. core. Since the advent of olefin polymerization catalysts in 1953, there have been three important milestones in the Ziegler-Natta catalytic system, metallocene catalytic system and late transition metal catalytic system in just over fifty years. Different polymerization methods will lead to completely different structures and properties of norbornene polymers obtained. Addition-...
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