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Rare earth catalyst and preparation method thereof and styrene syndiotactic polymerization method

A rare earth catalyst and catalyst technology, which are applied in the directions of organic chemistry methods, chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, etc., can solve the problems of high cost of catalysts and limited application, and achieve simple and feasible preparation methods. The effect of cost reduction and easy availability of raw materials

Active Publication Date: 2018-10-12
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, scandium is an expensive rare earth metal, which directly leads to the high cost of the catalyst, which limits its application in the polymerization industry.

Method used

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  • Rare earth catalyst and preparation method thereof and styrene syndiotactic polymerization method
  • Rare earth catalyst and preparation method thereof and styrene syndiotactic polymerization method
  • Rare earth catalyst and preparation method thereof and styrene syndiotactic polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The mononuclear rare earth catalyst in this example is an ethyl-bridged 2,5-dimethylpyrrole aniline dibenzyl scandium compound (2,5-Me 2 C 4 h 2 NCH 2 CH 2 NC 6 h 5 )Sc(CH 2 C 6 h 4 NMe 2 -o) 2 ; Hereinafter referred to as catalyst 1, its structural formula is as shown in formula 1:

[0037]

[0038] The concrete preparation method of this catalyst is as follows:

[0039] In the glove box, the Sc(CH 2 C 6 h 4 NMe 2 -o) 3 (224mg, 0.5mmol) was dissolved in 5mL of toluene, 2,5-Me 2 C 4 h 2 NCH 2 CH 2 NHC 6 h 5 (107 mg, 0.5 mmol) was dissolved in 5 mL of toluene, and the two solutions were mixed to obtain a yellow clear liquid. After reacting at room temperature for 15 hours, the solvent was sucked dry, and the residual yellow oil was washed with hexane (3 times, the amount of hexane was 5 mL each time). Then it was sucked dry under reduced pressure to obtain 0.23 g of light yellow powder, and the calculated molar yield was 85%.

[0040] The calc...

Embodiment 2

[0046] Catalyst (hereinafter referred to as catalyst 2) in the present embodiment, its structure is as shown in formula 2:

[0047]

[0048] The concrete preparation method of this catalyst is as follows:

[0049] In the glove box, the Y(CH 2 C 6 h 4 NMe 2 -o) 3 (246mg, 0.5mmol) was dissolved in 5mL of toluene, 2,5-Me 2 C 4 h 2 NSiMe 2 NHC 6 h 5 (122 mg, 0.5 mmol) was dissolved in 5 mL of toluene, and the two solutions were mixed in a Schlenk bottle to obtain a yellow clear liquid. The reaction bottle was removed from the glove box, and reacted in a pre-prepared 50°C oil bath for 5 hours, then the solvent was drained, and the residual yellow oil was washed with hexane (washing 3 times, the amount of hexane was 5 mL each time). Then it was sucked dry under reduced pressure, and recrystallized in a mixed solution of toluene and hexane to obtain 0.22 g of colorless crystals, and the calculated molar yield was 71%.

[0050] Characterization data for dimethylsilyl br...

Embodiment 3

[0054] The rare earth catalyst (hereinafter referred to as catalyst 3) of this embodiment is dimethylsilylmethylene bridged 2,5-dimethylpyrrole p-chloroaniline dibenzyl lanthanum compound (2,5-Me 2 C 4 h 2 NCH 2 SiMe 2 NC 6 h 4 Cl-p)La(CH 2 C 6 h 4 NMe 2 -o) 2 ; Its structure is as shown in formula 3:

[0055]

[0056] The concrete preparation method of this catalyst is as follows:

[0057] In the glove box, La(CH2 C 6 h 4 NMe 2 -o) 3 (542mg, 1.0mmol) was dissolved in 10mL of toluene, 2,5-Me 2 C 4 h 2 NCH 2 SiMe 2 NHC 6 h 4 (p-Cl) (293 mg, 1.0 mmol) was dissolved in 10 mL of toluene, and the two solutions were mixed to obtain a yellow clear liquid. After reacting at room temperature for 15 hours, the solvent was removed under reduced pressure, concentrated to about 1.0 mL, left to crystallize at room temperature, and 0.60 g of yellow cubic crystals were obtained. The calculated molar yield was 84%.

[0058] Characterization data of catalyst 3 dimethyl...

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Abstract

The invention relates to a rare earth catalyst and a preparation method thereof and a styrene syndiotactic polymerization method. The structural formula of the catalyst is shown in the description, wherein Ln is rare earth metal; R is alkyl or amido or halogen connected with the rare earth metal; B is alkyl with 1-10 carbon atoms or alkyl with 1-10 carbon atoms and several silicon atoms or alkyl with 1-10 carbon atoms and several halogen atoms; D is N or P or As; R' is hydrogen or methyl or ethyl or isopropyl or t-butyl; R'' is aryl or alkyl containing various substituent groups.

Description

technical field [0001] The invention relates to the field of high polymer catalysts, in particular to a rare earth catalyst, a preparation method thereof and a syndiotactic polymerization method for styrene. Background technique [0002] There are three types of polystyrene: atactic polystyrene (aPS), isotactic polystyrene (iPS) and syndiotactic polystyrene (sPS). Among them, syndiotactic polystyrene has a high melting point (270°C), fast crystallization speed, high elastic modulus, solvent resistance, good dimensional stability and excellent electrical properties, and is a special polymer material that has attracted wide attention. [0003] Syndiotactic polystyrene was first invented by Professor Ishihara of Idemitsu Chemical Co., Ltd., using titanium-based catalyst CpTiX 3 / MAO preparation, the disadvantage of this system is that syndiotactic polystyrene and atactic polystyrene will be produced at the same time. In 2004, Hou Zhaomin’s research group from RIKEN and France...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/08C08F4/52C07F5/00C07F7/10
CPCC07B2200/07C07F5/00C07F7/10C08F112/08C08F4/52
Inventor 罗云杰李敏王朝磐牟泽怀
Owner NINGBO UNIV
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