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CGC type aminofluorene rare-earth metal catalyst and preparation method and application thereof

A technology of rare earth metals and catalysts, which is applied in the field of catalysts and can solve the problems that the application of preparation methods has not yet been reported.

Inactive Publication Date: 2019-01-22
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the catalysts with fluorene as a ligand are metallocene catalysts, and the CGC type amine fluorene rare earth metal organocatalyst (non-metallocene), preparation method and its application in polymerization reactions involved in the present invention have not yet been reported

Method used

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  • CGC type aminofluorene rare-earth metal catalyst and preparation method and application thereof
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  • CGC type aminofluorene rare-earth metal catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] (1) Preparation of aminofluorene ligand

[0078]

[0079] Step 1: First, add 8.35ml (20mmol, 2.4mol / L) of n-butyllithium dropwise to 3.33g (20mmol) of fluorene in tetrahydrofuran at -70°C under a nitrogen atmosphere to react for 2 hours to obtain mixture a; secondly , at -7°C, the mixture was added dropwise to the tetrahydrofuran solution of dichlorodimethylsilane and reacted for 5 hours to obtain the mixture b; finally, the reaction solution was drained, extracted three times with n-hexane, and the extract was drained to obtain The product of the first step is 3.188g, and the yield is 61.3%.

[0080] The second step: under the protection of nitrogen at room temperature, 0.8 g (10 mmol) of tert-butylamine and 4 g (4 mmol) of triethylamine were respectively added to the tetrahydrofuran solution of the first step product 2.6 g (10 mmol) and stirred for 5 h; the reaction solution was drained, After extraction with n-hexane, the extract was concentrated and transferred ...

Embodiment 2

[0085] Preparation of CGC-type Aminofluorene Lutetium Catalyst

[0086]

[0087] First, in the glove box, 591 mg (2 mmol) of the aminofluorene ligand was added to a round-bottomed flask, and 10 ml of n-hexane was used as a solvent to fully dissolve; secondly, Lu(CH 2 SiMe 3 ) 3 thf 2 1.16g (2mmol) was dissolved in 3mL of n-hexane, and the n-hexane solution in which the aminofluorene ligand was dissolved was added dropwise to the n-hexane solution in which the metal source was dissolved, and stirred at room temperature for 3 hours, a yellow solid precipitated; finally, centrifuged to obtain a yellow The solid was washed three times with cold n-hexane to obtain 1.08 g of aminofluorene catalyst with a yield of 75.4%.

Embodiment 3

[0089] Preparation of CGC type amine fluorene yttrium catalyst

[0090]

[0091] First, in the glove box, 591 mg (2 mmol) of the aminofluorene ligand was added to a round-bottomed flask, and 10 ml of n-hexane was used as a solvent to fully dissolve it; secondly, Y(CH 2 SiMe 3 ) 3 thf 2 1g (2mmol) was dissolved in 3mL of n-hexane, and the n-hexane solution in which the aminofluorene ligand was dissolved was added dropwise to the n-hexane solution in which the metal source was dissolved, and stirred at room temperature for 3 hours, a yellow solid precipitated; finally, centrifuged to obtain a yellow solid , washed three times with cold n-hexane to obtain 1.09 g of aminofluorene catalyst with a yield of 85.7%.

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Abstract

The invention discloses a CGC type aminofluorene rare-earth metal catalyst and a preparation method and application thereof, and belongs to the technical field of catalysts. The catalyst has three structural formulas. The novel CGC aminofluorene rare-earth metal catalyst can catalyze the homopolymerization or copolymerization of olefins, alkynes, CO2 and polar monomers such as 2-vinylpyridine, 4-vinylpyridine, epoxyalkane or lactone. When the catalyst is applied in catalyzing the polymerization of isoprene, the content of cis 1,4 in the obtained polyisoprene reaches up to 96%. In addition, when the catalyst is applied in catalyzing the polymerization of styrene, syndiotactic polystyrene with rrrr = 100% is obtained. Especially when the catalyst is applied in the polymerization of myrcene,the content of cis 1,4 in the obtained polymyrcene reaches up to 100%. The catalyst of the invention can polymerize polar monomers and has good catalytic activity and selectivity.

Description

technical field [0001] The invention relates to a CGC-type amine fluorene rare earth metal catalyst, a preparation method and an application, and belongs to the technical field of catalysts. Background technique [0002] As we all know, polyolefin materials are the most consumed synthetic resins, and the demand for polyolefins in countries around the world continues to increase. Because polyolefin materials have excellent properties, such as: good mechanical properties, processing properties, medical properties, thermal properties, corrosion resistance, etc., polyolefin materials have a wide range of uses. [0003] Polyolefin obtained by olefin coordination polymerization is the largest proportion of polymer materials, which has many excellent properties, such as good processing performance, mechanical properties, electrical insulation, thermal performance, corrosion resistance, etc., widely used in industry, Agriculture, national defense, transportation, medical treatment ...

Claims

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Application Information

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IPC IPC(8): C08F136/08C08F110/14C08F112/08C08F4/54C08G63/08C08G63/84
CPCC08F110/14C08F112/08C08F136/08C08G63/08C08G63/823C08F4/545
Inventor 李晓芳郭歌严新稳吴晓路
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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