Method for preparing butene oligomer
A technology of oligomers and butene, which is applied in the field of preparing butene oligomers, can solve problems such as pollution, catalyst activity degradation, difficulty in preparing polymers with high molecular weight, etc., and achieve the effect of solving product quality and reducing toxicity
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[0053] 1. The preparation method of butene oligomer
[0054] One embodiment of the present invention provides a method for preparing a butene oligomer, comprising polymerizing a compound comprising a halogenated hydrocarbon solvent, a nonpolar hydrocarbon solvent, and an isobutylene monomer in the presence of an organometallic catalyst represented by Formula 1. Solution oligomerization steps.
[0055] The method for producing a butene oligomer of the present invention is characterized in that the oligomerization step is performed by using a mixture solvent containing a halogenated hydrocarbon solvent and a nonpolar hydrocarbon solvent. In this case, an effect of reducing the toxicity of the halogenated hydrocarbon solvent can be achieved when compared with the case of using the halogenated hydrocarbon solvent alone.
[0056] In addition, the polarity of the solvent affects the reactivity during the polymerization of butene oligomers, and by mixing a halogenated hydrocarbon so...
preparation Embodiment 1
[0142]
[0143] In the glove box, 100 mg of Al(OH) 2 (OAc) (purchased from Sigma-Aldrich) was placed in the bottle together with a magnetic rod, and 2 ml of acetonitrile solvent was added thereto. Add 3 equivalents of [Et 3 Si] + [B(C 6 f 5 ) 4 ] (available from Asahi Glass Co.) metal precursor, and 3 ml of acetonitrile solvent was also added thereto for dissolution. While stirring, [Et] dissolved in acetonitrile was slowly added to the Al precursor solution 3 Si] + [B(C 6 f 5 ) 4 ]. Then, stirring was performed at room temperature for 5 hours. After removing all solvents in vacuo, washes were performed with benzene and hexane. The remaining substance was sufficiently dried in vacuum to obtain a powder type transition metal complex.
Embodiment 1
[0145]
[0146] Prepare the Andrew's glass pressure reactor depleted of moisture and oxygen. 20 g of isobutylene were added through a line connected to the isobutylene storage tank and Andrew's glass. A mixture solvent of 20 ml of hexane and 60 ml of dichloromethane (DCM) was used as a solvent after being stored in molecular sieves to remove moisture, and after calculating the monomer concentration in the reactant (total solution of compound, TSC), using The syringe joins from the top of the Andrew glass. After completion of solvent and monomer addition, the Andrew glass was moved into a water bath and the temperature was set to a polymerization temperature of 30°C.
[0147] Based on the total weight of monomers, 0.01% by weight of the catalyst of Preparation Example 1 stored in a glove box at low temperature was weighed and dissolved in DCM solvent. The resulting solution was transferred to a pressure syringe and removed from the glove box. The reactor was pressurized t...
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