1-octene, 1-decene, 1-dodecene ternary copolymer and lubricant composition containing same
A dodecene terpolymer, dodecene technology, applied in lubricating compositions, petroleum industry, base materials, etc., can solve the problem of undisclosed selective synthesis method, insufficient flow point, low molecular weight polymer and other problems, to achieve the effect of excellent oxidation stability
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[0110] Next, the present invention will be described in more detail using examples, but the present invention is not limited to these examples.
[0111] The evaluation of the physical properties of the α-olefin polymer was carried out by the following methods.
[0112] (1) Flow point
[0113] Measured in accordance with JIS K 2269.
[0114] (2) Kinematic viscosity and viscosity index
[0115] The kinematic viscosity is measured according to JIS K 2283. Viscosity index is calculated from kinematic viscosity according to JIS K 2283.
[0116] (3) Number average molecular weight and molecular weight distribution (Mw / Mn)
[0117] Using JASCO GPC-900 (column; TOSOH TSK-GEL MULTIPORE HXL-M (2 pieces) + Shodex KF801 (1 piece)) device, under the conditions of solvent; tetrahydrofuran, temperature; 40°C, and polystyrene conversion Get it.
[0118] (4) Meso triad fraction (mm)
[0119] Using the method described in [Macromolecules24, 2334 (1991); Polymer, 30, 1350 (1989)], using ...
manufacture example 1
[0134] Production Example 1 [Production of (1,1'-dimethylsilylene)(2,2'-dimethylsilylene)-bis(cyclopentadienyl)zirconium dichloride]
[0135] About 13.8 g (600 mmol) of metallic Na and 400 ml of dry THF (tetrahydrofuran) were added to a 1000 ml three-necked flask replaced with nitrogen, and stirred at 0°C. After 5 minutes, 1 to 2 ml of cyclopentadiene was added dropwise thereto, and when generation of hydrogen was completed, 1 to 2 ml of cyclopentadiene was added again, and the process was repeated to add a total of 50 ml (600 mmol) of cyclopentadiene. The reaction solution changed from colorless and transparent to light pink. After THF was distilled off under reduced pressure, the crystals were washed twice with hexane and dried under reduced pressure to obtain cyclopentadienyl sodium as a pink powder.
[0136] 457 ml of THF was added to 43.0 g (480 mmol) of cyclopentadienyl sodium at 0° C., followed by stirring. After cooling to -78°C, 29.2ml (480mmol) of dichlorodimethyls...
Embodiment 1-1
[0143] A stainless steel autoclave with an internal volume of 1 liter was fully dried and replaced with nitrogen, and 146 ml of 1-dodecene, 183 ml of 1-decene, and 71 ml of 1-octene were added, followed by addition of triisobutylaluminum 0.2 mmoles, the temperature was raised to 105°C. Put into the catalyst mixed solution prepared separately (in a 10 ml glass Schlenk bottle, add 0.1 mmol of triisobutylaluminum (2 mmol / ml toluene solution; 0.05 ml) under nitrogen atmosphere, obtain in Production Example 1 (1,1'-dimethylsilylene)(2,2'-dimethylsilylene)-bis(cyclopentadienyl)zirconium dichloride 10 μmol (10 μmol / mL of toluene solution; 1 mL) and powdered N, N-dimethylanilinium tetrakis (pentafluorophenyl) borate 0.012 mmol (11.5 mg), after stirring at room temperature for about 1 minute, add 1 -0.5 ml of octene, and further stirred at room temperature for 1 hour) After 1 ml of hydrogen, 0.05 MPaG was introduced to initiate polymerization. After 60 minutes at 105°C, add 1 ml of ...
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