Poly-1-butene and preparation method thereof
A technology of butene and olefin, applied in the field of preparation of poly-1-butene, can solve the problem of low isotacticity and achieve the effect of high catalyst activity
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preparation example Construction
[0014] The invention provides a method for preparing poly-1-butene, the method comprising: under the condition of olefin solution polymerization, contacting a monomer containing 1-butene with an olefin catalyst, and the olefin catalyst contains a solid component , an external electron donor compound and an organoaluminum compound, the solid component contains a carrier and a titanium compound and an internal electron donor compound loaded on the carrier; in the monomer containing 1-butene, 1-butene The content of alkene is 60-100 mol%, and described external electron donor compound is as shown in formula (1):
[0015]
[0016] Among them, R 2 and R 3 are not the same; and R 1 -R 3 each independently for C 1 -C 6 Straight chain or branched chain alkyl, C 3 -C 8 Cycloalkyl, C 6 -C 14 Aryl or C 5 -C 14 heteroaryl.
[0017] According to the method of the present invention, the olefin solution polymerization reaction conditions may include: the temperature is 0-80°C,...
preparation example 1
[0061] This preparation example is used to illustrate the external electron donor compound and its preparation method of the present invention.
[0062] Add 150 mL of methyl tert-butyl ether, 100 mmol of magnesium powder, and 20 mmol of chloroisopropane into a three-necked flask. At room temperature, iodine is added to initiate the reaction to generate the Grignard reagent. After the reaction is stable, slowly add a mixed solution of 80 mmol isopropane chloride and 100 mmol methyltrimethoxysilane dropwise through the dropping funnel. After 30 minutes, the dropwise addition is completed, and the reaction is started at 80° C. for 3 hours. After the reaction was completed, filter through a G4 funnel, wash the filtered solid residue twice with tetrahydrofuran repeatedly, and collect the filtrate. Use a rotary evaporator to evaporate the THF solvent, distill under reduced pressure, collect fractions at 62-65°C / 100Pa, and obtain a product weighing 5.7g with a purity of 97.5%. The ...
preparation example 2
[0064] This preparation example is used to illustrate the external electron donor compound and its preparation method of the present invention.
[0065] Add 150 mL of methyl tert-butyl ether, 100 mmol of magnesium powder, and 20 mmol of chloroisobutane into a three-necked flask. Under normal temperature conditions, iodine is added to initiate the reaction to generate Grignard reagent. After the reaction is stable, slowly add a mixed solution of 80 mmol chloroisobutane and 100 mmol methyltrimethoxysilane dropwise through the dropping funnel, and finish the dropwise addition after 30 minutes, start heating and react at 80° C. for 3 h. After the reaction was completed, filter through a G4 funnel, wash the filtered solid residue twice with tetrahydrofuran repeatedly, and collect the filtrate. Use a rotary evaporator to evaporate the THF solvent, distill under reduced pressure, collect fractions at 65-69° C. / 100 Pa, and obtain a product weighing 6.8 g with a purity of 98.5%. The ...
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