Spherical magnesium halide adduct and preparation method and application thereof
A magnesium halide and adduct technology, applied in the direction of magnesium organic compounds, etc., can solve the problem that the isotacticity needs to be further improved
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[0044] The present invention also provides a method for preparing the spherical magnesium halide adduct, the method comprising:
[0045] (1) MgXY is mixed with alcohol and compound E and heated to obtain a liquid magnesium halide adduct;
[0046] (2) emulsifying the liquid magnesium halide adduct in the presence of an inert liquid medium, and rapidly cooling the emulsified product to obtain spherical magnesium halide adduct particles,
[0047] In MgXY, X is chlorine or bromine, Y is chlorine, bromine, C 1 -C 14 Straight chain or branched chain alkyl, C 6 -C 14 Substituted or unsubstituted aryl, C 1 -C 14 straight-chain or branched-chain alkoxy and C 6 -C 14 One of the substituted or unsubstituted aryloxy groups;
[0048] Described alcohol is general formula R (OH) r The compound shown, R in the general formula is C 1 -C 20 Hydrocarbyl, r is an integer greater than 1;
[0049] Compound E is a hydroxybenzoic acid compound or a hydroxybenzoate compound shown in formul...
Embodiment 1
[0082] This example is used to illustrate the spherical magnesium halide adduct and its preparation method according to the present invention.
[0083] In a 500mL reactor, add 150mL of white oil, 30g of magnesium chloride, 50mL of absolute ethanol and 1mL of ethyl 2-hydroxybenzoate, and raise the temperature to 120°C while stirring. After 2 hours of constant temperature reaction, the mixture was pressed into 300 mL of methyl silicone oil preheated to 120° C., and stirred at high speed (1600 rpm) for 30 minutes to disperse for emulsification. Then, the emulsified product was injected into 2 L of hexane pre-cooled to -30° C. with nitrogen pressure to solidify and form. The liquid was removed by filtration, the solid was washed 5 times with 300 mL of hexane, and dried in vacuo to obtain a spherical magnesium halide adduct. The composition of this magnesium halide adduct is: Mg=10.9wt%, ethanol=55.7wt%, 2-hydroxybenzoic acid ethyl ester=1.43wt%, adopt the particle morphology of o...
Embodiment 2
[0085] This example is used to illustrate the application of spherical magnesium halide adducts according to the present invention in the preparation of olefin polymerization catalysts.
[0086] (1) In a 300mL glass reaction flask, under nitrogen protection conditions, add 18mL of hexane and 90mL of titanium tetrachloride successively, cool to -20°C, add 8.0g of the spherical magnesium halide adduct prepared in Example 1, and Stirring was maintained at -20°C for 30 minutes. Afterwards, the temperature was slowly raised to 110° C., and 1.5 mL of diisobutyl phthalate was added during the temperature rise. After reacting at a constant temperature of 110° C. for 30 minutes, the liquid was filtered off. Add 80 mL of titanium tetrachloride, raise the temperature to 120° C., and filter the liquid after maintaining at 120° C. for 30 minutes; repeat the above operation once. Finally, the obtained solid was washed 5 times with 60° C. hexane (the amount of hexane was 80 mL / time); and t...
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