An aminophenol-based phosphorus ligand and its application in ethylene polymerization and oligomerization
A technology for ethylene polymerization and aminophenol, which is applied in the direction of organic compound/hydride/coordination complex catalysts, hydrocarbons, hydrocarbons, etc., and can solve the problem that the selectivity of 1-octene does not reach the ethylene trimerization process, etc.
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[0024] refer to figure 1 , the present invention specifically adopts the following embodiments: the ligand is a phosphorus-containing derivative based on aminophenol, and its structural formula is as follows:
[0025]
[0026] in:
[0027] In the aminophenol structure, the amino group is in the ortho, meta or para position of the phenolic hydroxyl group;
[0028] R 1 It is an alkyl group, cycloalkyl group, alkoxy group, or aryl group with no more than 10 carbon atoms;
[0029] R 2 It is an alkyl, cycloalkyl, aryl, or alkoxy group with less than 10 carbon atoms;
[0030] R 3 Alkyl, cycloalkyl, aryl, alkoxy with less than 10 carbon atoms
[0031] The method of use: the complex or mixture formed by prefabrication or on-site preparation of the phosphorus ligand and the transition metal compound, the positive ions of the transition metal salt include Cr(II), Cr(III), Ni(II), Fe( II), Co(III), Pd(II), Zr(II), Zr(IV), Pt(II), among which Cr(II), Cr(III), Ni(II), Fe(II) Pd a...
Embodiment 1
[0040] Preparation of multisite phosphorous ligand 1
[0041] In the structure of ligand 1, R 1 , R 2 , R 3 Both are hydrogen, and the amino group is in the ortho position to the hydroxyl group. Its structure is as figure 2 shown.
[0042]Under the protection of high-purity nitrogen, add 5.8mL of diphenylphosphorus chloride and 40mL of tetrahydrofuran into the flask. After fully stirring and dissolving, add 4.5mL of triethylamine. After stirring for half an hour, the temperature is lowered to 0°C, and the solution is added dropwise. Add a solution of o-aminophenol (1.24g of o-aminophenol dissolved in 10mL of tetrahydrofuran), and continue stirring at 0°C for half an hour after the addition is complete. The reaction was continued for 12 hours after cooling down and naturally warming to room temperature. The mixture was filtered to remove solids, and the obtained filtrate was rotary evaporated to remove the solvent to obtain a crude product. The crude product was recrys...
Embodiment 2
[0044] Ligand 1 catalyzes ethylene oligomerization
[0045] The 500mL stainless steel autoclave that was continuously vacuum-dried at 80°C for more than 2 hours was replaced with high-purity nitrogen for 3 times, and then evacuated and replaced with ethylene for 3 times. Inject 150 mL of toluene into the kettle under the condition of maintaining a slight positive pressure in the kettle, start stirring, add 7.0 mg of chromium acetylacetonate dissolved in toluene solution and 14.5 mg of Ligand 1 dissolved in toluene solution, add 8.0 mL of cocatalyst after 5 minutes Methylalumoxane (10% solution in toluene). Inject ethylene at 50°C to make the pressure in the kettle reach and maintain 3MPa, measure the amount of ethylene with a mass flow meter, and stir at a speed of 700rpm. After 30 minutes of reaction, the ethylene feed was cut off, the temperature of the autoclave was lowered to 0°C, and then the pressure was released to normal pressure, and the catalyst and polymer were rem...
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