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Poly(ethylene-r-norbornene/ethylene) segmented copolymer synthesized by utilizing 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 problem of poor catalyst tolerance, few types, difficult issues of industrial production

Active Publication Date: 2019-03-15
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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  • Poly(ethylene-r-norbornene/ethylene) segmented copolymer synthesized by utilizing chain shuttling method
  • Poly(ethylene-r-norbornene/ethylene) segmented copolymer synthesized by utilizing chain shuttling method
  • Poly(ethylene-r-norbornene/ethylene) segmented copolymer synthesized by utilizing 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 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.

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

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 invention discloses a poly(ethylene-r-norbornene / ethylene) segmented copolymer synthesized by utilizing a chain shuttling method. The preparation method comprises the following steps: preparing amixed catalyst; adding polymerization monomers and regulating a polymerization temperature; adding a promoter and a chain shuttling agent; adding a catalyst for performing chain shuttling polymerization; terminating the polymerization reaction; and precipitating and drying the polymer solution. Diethyl zinc is selected as the chain shuttling agent, an ethylene / norbornene random chain segment synthesized from a Rac-ethyl bridged zirconium dichloride diindene catalyst serves as a soft segment, a polyethylene segment synthesized from a Rac-3-tert-butyl substituted methyl bridged zirconium dichloride diindene catalyst serves as a hard segment, and the poly(ethylene-r-norbornene / ethylene) segmented copolymer is synthesized for the first time. The method and the substance are not reported in many technologies, and conditions are provided for realizing wide application of the novel 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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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
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