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Synthesis of poly(ethylene-r-norbornene/ethylene) multi-block copolymers by chain shuttling method

A technology of multi-block copolymer and norbornene, which is applied in the field of synthesizing poly(ethylene-r-norbornene/ethylene) multi-block copolymer by chain shuttling, can solve the problems of few types, poor polymer performance, Problems such as poor catalyst tolerance

Active Publication Date: 2021-03-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The rare earth metal catalysts of the III subgroup have also reported a series of successful examples of chain shuttling. Due to the poor performance of the obtained polymers and the poor tolerance of the catalysts, it is difficult to industrialize production.
The main problem at present is that there are few types of products for polymers prepared by chain shuttling

Method used

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  • Synthesis of poly(ethylene-r-norbornene/ethylene) multi-block copolymers by chain shuttling method
  • Synthesis of poly(ethylene-r-norbornene/ethylene) multi-block copolymers by chain shuttling method
  • Synthesis of poly(ethylene-r-norbornene/ethylene) multi-block copolymers by chain shuttling method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] In this example, the polymerization temperature is 50°C, the ethylene pressure is 1 atm, the molar content of diethyl zinc is 10 times that of the mixed catalyst, and the mixed catalyst Rac-ethyl bridged dichlorodiindene zirconium A and Rac-3-tert-butyl Chain shuttling polymerization with a polymerization time of 6 minutes under the condition that the molar ratio of substituted methine bridged dichlorodiindene zirconium B is 3:1.

[0047] Chain shuttling polymerization in this embodiment includes the following steps:

[0048] (1) Weigh and equip the chain shuttling catalyst: weigh Rac-ethyl bridged diindene zirconium dichloride and Rac-3-tert-butyl substituted methine bridged diindene dichloride with an analytical balance in the glove box The zirconium mixed catalyst, whose molar ratio is 3:1, is fully dissolved in toluene, and is reserved for later use.

[0049] (2), adding of polymerized monomer and regulating polymerization temperature: adding the comonomer norborne...

Embodiment 2

[0057] In this example, the polymerization temperature is 50°C, the ethylene pressure is 1 atm, the molar content of diethyl zinc is 10 times that of the mixed catalyst, and the mixed catalyst Rac-ethyl bridged dichlorodiindene zirconium A and Rac-3-tert-butyl Chain shuttling polymerization with a polymerization time of 15 minutes under the condition that the molar ratio of substituted methine bridged dichlorodiindene zirconium B is 3:1.

[0058] Chain shuttling polymerization in this embodiment includes the following steps:

[0059] (1) Weigh and equip the chain shuttling catalyst: weigh Rac-ethyl bridged diindene dichloride zirconium and Rac-3-tert-butyl substituted methine bridged dichlorobisindene with an analytical balance in the glove box The zirconium mixed catalyst, whose molar ratio is 3:1, is fully dissolved in toluene, and is reserved for later use.

[0060] (2), the addition of polymerized monomers and the adjustment of the polymerization temperature: the comonome...

Embodiment 3

[0067] In this example, the polymerization temperature is 70°C, the ethylene pressure is 1 atm, the molar content of diethyl zinc is 15 times that of the mixed catalyst, and the mixed catalyst Rac-ethyl bridged dichlorodiindene zirconium A and Rac-3-tert-butyl Chain shuttling polymerization with methine bridged dichlorodiindene zirconium B molar ratio of 1:1 and polymerization time of 10 min.

[0068] Chain shuttling polymerization in this embodiment includes the following steps:

[0069] (1) Weigh and equip the chain shuttling catalyst: weigh Rac-ethyl bridged diindene zirconium dichloride and Rac-3-tert-butyl substituted methine bridged diindene dichloride with an analytical balance in the glove box The zirconium mixed catalyst, whose molar ratio is 1:1, is fully dissolved in toluene, and is reserved for later use.

[0070] (2), adding of polymerized monomer and regulating polymerization temperature: adding the comonomer norbornene dissolved in toluene in the polymerization...

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Abstract

The present invention proposes to utilize the chain shuttling method to synthesize poly(ethylene-r-norbornene / ethylene) multi-block copolymers, including the addition of mixed catalysts, the addition of polymerized monomers and the adjustment of polymerization temperature, the addition of co-catalysts and chain shuttling agents, and the addition of Catalysts carry out the process of chain shuttling polymerization, termination of polymerization reaction and precipitation and drying of polymer solution. By choosing diethylzinc as the chain shuttling agent, the ethylene / norbornene random segment was synthesized as the soft segment, and the Rac-3-tert-butyl substituted methine bridge was synthesized with the catalyst of Rac-ethyl bridged diindene zirconium dichloride The poly(ethylene-r-norbornene / ethylene) multi-block copolymer was synthesized for the first time by using the dichlorobisindene zirconium catalyst to synthesize the polyethylene segment as a hard segment. The method and substance have not been reported in many technologies, which provides conditions for realizing the wide application of this new material.

Description

technical field [0001] The invention relates to the technical field of preparation of poly(ethylene-r-norbornene / ethylene) multi-block copolymers synthesized by a chain shuttling method, specifically refers to the selection of ethylene and norbornene comonomers with relatively large selectivity and structure A preparation method for synthesizing poly(ethylene-r-norbornene / ethylene) multi-block copolymer elastomer materials with two similar zirconocene metal catalysts. Background technique [0002] Since Ziegler's pioneering work on olefin coordination polymerization, the scientific research and industrial application of olefin coordination polymerization have flourished. Polyolefins synthesized by coordination polymerization have become the world's largest and most widely used polymer materials. Because polyolefin has the characteristics of low relative density, good chemical resistance and water resistance; good mechanical strength and electrical insulation, it can be used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F297/06C08F210/02C08F232/08C08F4/6592C08F2/38
CPCC08F210/02C08F297/06C08F232/08C08F4/65927C08F2/38
Inventor 潘莉高欢李悦生
Owner TIANJIN UNIV