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Rare earth complex and its preparation method, polymerization catalytic system and its preparation method, polymer preparation method

A rare earth complex and complex technology are applied in the preparation of polymers, rare earth complexes and their preparation, catalytic systems for polymerization and their preparation fields, and can solve the problem of polystyrene random and high syndiotactic styrene segments Difficulty in obtaining copolymers

Active Publication Date: 2015-08-05
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2000, the Wakatsuki research group reported that samarium complexes catalyzed the polymerization of styrene with very high activity, but the obtained polystyrene was random
For example, some coordination catalysts based on rare earth metals or transition metals have been reported to obtain highly regular polymers by catalyzing styrene-butadiene copolymerization and styrene-isoprene copolymerization, but with high inter- Copolymers with regular styrene segments are very difficult to obtain, so the synthesis of copolymers with highly regular styrene segments by coordination polymerization is extremely challenging in academia and industry, but at the same time is very promising

Method used

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  • Rare earth complex and its preparation method, polymerization catalytic system and its preparation method, polymer preparation method
  • Rare earth complex and its preparation method, polymerization catalytic system and its preparation method, polymer preparation method
  • Rare earth complex and its preparation method, polymerization catalytic system and its preparation method, polymer preparation method

Examples

Experimental program
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preparation example Construction

[0040] Correspondingly, the present invention also provides a preparation method of a rare earth complex, comprising the following steps: 2 Under protection, the restricted geometry ligand R 1 H-R 2 -(3-R 3 -4-R 4 -5-R 5 -6-R 6 )C 5 N is dissolved in tetrahydrofuran at -78°C to 0°C, and a n-hexane solution of n-butyllithium with a concentration of 1.0 to 2.0mol / L is added in sequence, and the chemical formula is LnCl 3 (thf) n (n=2~3.5) rare earth trichloride and single anion ligand, and described single anion ligand is CH 2 SiMe 3 、CH(SiMe 3 ) 2 , o-NMe 2 -CH 2 C 6 h 4 , 1,3-C 3 h 5 , 1,3-C 3 h 4 (Me) or 1,3-C 3 h 3 (SiMe 3 ) 2 ; 1 is the fluorenyl derivative C 13 A 8 , Indenyl derivatives C 9 A 6 or cyclopentadienyl derivative C 5 A 4 , A is selected from hydrogen, aliphatic hydrocarbon group or aromatic hydrocarbon group; R 2 selected from methylene, or ethyl or dimethylsilyl; R 3 selected from hydrogen, methyl, ethyl, isopropyl, tert-butyl or...

Embodiment 1

[0055] The preparation of embodiment 1 complex 1

[0056]

[0057] At -40°C, add a 1.0mol / L n-butyllithium solution in n-hexane (1.2mL, 1.2mmol) dropwise to 1-(2-pyridyl)-tert-butyl-cyclopentadiene (0.24g, 1.2mmol) in tetrahydrofuran (20mL). After the reaction solution reacted at this temperature for 1 hour, the ScCl 3 (thf) 3 (0.44g, 1.2mmol) was added in the above-mentioned reaction liquid, after reacting for 4 hours, LiCH 2 SiMe 3 (0.23g, 2.4mmol) was added, and after reacting at room temperature for 4 hours, the solvent was removed in vacuo, the residue was extracted with hexane, and the hexane solution was concentrated to obtain 0.26g of red crystal complex 1 with a yield of 54%. Elemental analysis target molecular formula is C 26 h 46 NOSi 2 Sc (%): C, 63.75; H, 9.47; N, 2.86.

Embodiment 2～5

[0058] The preparation of embodiment 2~5 complex 2-5

[0059] Change the reactant rare earth trichloride, other conditions and steps are the same as the complex preparation example 1, and the obtained restricted geometry configuration rare earth alkyl complexes 2-5 and the results are shown in Table 1:

[0060] Table 1 Constrained Geometry Rare Earth Alkyl Complexes 2-5 Prepared in Examples 2-5

[0061] Complex

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Abstract

The invention provides a rare earth complex and a preparation method of the rear earth complex. In the method, the synthesis is simple, and the yield reaches up to 45%-67%. The invention also provides a catalysis system for polymerization and a preparation method of the catalysis system. The invention also provides a preparation method of polystyrene. According to the preparation method of the polystyrene, the highest monomer conversion rate is 100%, the highest activity is 1.25*107g molLn-1h-1, the highest syndiotacticity (rrrr) of the synthesized polystyrene is 100%, and the number-average molar mass is 46,000-1,000,000, the lowest molecular weight distribution is 1.20. The polymerization reaction of butadiene and styrene is catalyzed by the catalysis system for polymerization, and the copolymer is characterized in that the polystyrene chain segment is of a syndiotacticity structure; the polybutadiene chain segment is mainly of a cis-1, 4-structure, and reaches 99.3%; the polyisoprene chain segment obtained by the polymerization reaction of the styrene and the isoprene catalyzed by the catalysis system for polymerization is mainly of a 3, 4-strcture and reaches 73.5%.

Description

technical field [0001] The invention relates to the technical field of catalysts, more specifically, to a rare earth complex and a preparation method thereof, a catalytic system for polymerization and a preparation method thereof, and a polymer preparation method. Background technique [0002] Polystyrene is divided into atactic polystyrene, syndiotactic polystyrene, and isotactic polystyrene according to different stereo configurations. The synthesis of polystyrene is mainly realized by free radical polymerization, anionic polymerization, cationic polymerization and Ziegler-Natta catalyst catalyzed polymerization. Traditional free radical polymerization, anionic polymerization and cationic polymerization mainly obtain atactic polystyrene, while Ziegler-Natta catalyst catalyzed styrene polymerization mainly obtains isotactic polystyrene. Compared with the uncontrollable selectivity of anionic polymerization, coordination polymerization has obvious advantages in controlling ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00C07F5/00C08F4/54C08F4/52C08F112/08C08F212/08C08F236/10
Inventor 崔冬梅潘玉鹏
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI