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Polysiloxane functionalized ethylene-norbornene copolymer and preparation method thereof

A polysiloxane and norbornene technology, applied in the field of copolymers, can solve the problems of low content, low copolymerization activity of comonomers and the like

Active Publication Date: 2021-01-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The design of the comonomer reduces the poisonous effect of the siloxane component on the catalytic system to a certain extent, but the copolymerization activity of the comonomer is low, and the siloxane component in the alkoxysilane-olefin random copolymer low content in

Method used

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  • Polysiloxane functionalized ethylene-norbornene copolymer and preparation method thereof
  • Polysiloxane functionalized ethylene-norbornene copolymer and preparation method thereof
  • Polysiloxane functionalized ethylene-norbornene copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] (1) A 50mL flask with a magnetic stirrer is vacuum-filled three times to make it full of inert atmosphere, add 5mL toluene, 3.33g (27.5mmol) vinyl norbornene and 50ppm Karstedt catalyst solution (platinum The mass concentration was 2%), and the temperature was controlled at 20° C. and stirred for 2 h. Then slowly add 2.6g (27.5mmol) dimethylchlorosilane, and continue to stir the reaction for 24h. The resulting product was distilled under reduced pressure to obtain 4.8 g of a colorless oily liquid product with a yield of 81%.

[0069] (2) A 100mL flask equipped with a magnetic stirrer was vacuum-filled three times with nitrogen to fill it with an inert atmosphere. Add 4.9g (22.5mmol) hexamethylcyclotrisiloxane and 10mL tetrahydrofuran, and then add 9mL A solution of n-butyllithium / hexane (2.5M) initiated the ring-opening polymerization. The temperature was controlled at 0° C. and the reaction was stirred for 2 h, and then 4.6 g (22.5 mmol) of the chlorosilane capping a...

Embodiment 2

[0073] (1) Repeat step (1) in Example 1.

[0074] (2) A 100mL flask equipped with a magnetic stirrer was vacuum-filled three times with nitrogen to fill it with an inert atmosphere, and then 10.5g (22.5mmol) of trifluoropropylmethylcyclotrisiloxane and 10mL of tetrahydrofuran were added , and then 9 mL of n-butyllithium / hexane solution (2.5 M) was added to initiate ring-opening polymerization. The temperature was controlled at 0° C. and the reaction was stirred for 2 hours, and then 4.6 g of the chlorosilane capping agent prepared in step (1) was added, and the capping time was 24 hours. After washing with deionized water and n-hexane three times, drying with anhydrous magnesium sulfate and rotary evaporation to remove the solvent, 13.9 g of colorless liquid product was obtained, which was polytrifluoropropylmethylsiloxane functionalized norbornene monomer . The yield was 88%. It can be seen from the characterization of the hydrogen NMR spectrum that in the prepared monomer...

Embodiment 3

[0078] The preparation process is the same as in Example 2, except that the addition amount of polytrifluoropropylmethylsiloxane functionalized norbornene monomer in step (3) is 4.2g (120mmol / L), and 2.4g of the product is obtained.

[0079] From further analysis, it can be seen that the polymerization activity of the copolymerization reaction is as high as 2.88×10 7 g / (mol·h). The content of polytrifluoropropylmethylsiloxane functionalized norbornene monomer in the copolymer is 8.6 mol%. The copolymer had a weight average molecular weight of 46.9 kg / mol as determined by GPC analysis.

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Abstract

The invention relates to a polysiloxane functionalized ethylene-norbornene copolymer and preparation method thereof. The structural general formula of the polysiloxane functionalized ethylene-norbornene copolymer is shown as the following formula (I-1) or (I-2), in the formula, R1 is selected from C1-C8 alkyl, C1-C8 fluorine-containing alkyl or phenyl, and R2 is selected from C1-C8 alkyl; whereinx is a natural number ranging from 100 to 10000, y is a natural number ranging from 10 to 300, and a is a natural number ranging from 3 to 90. The preparation method comprises three steps of hydrosilylation, anionic ring-opening polymerization and coordination copolymerization, and the preparation method avoids the toxic action of the strong polarity of polysiloxane on a transition metal catalystcommonly used in olefin polymerization under the condition of high polysiloxane content; the polysiloxane content and the weight-average molecular weight in the prepared polysiloxane functionalized ethylene norbornene copolymer can be adjusted in a large range, and the polysiloxane functionalized ethylene norbornene copolymer can be used as a novel polyolefin polysiloxane hybrid thermoplastic elastomer through structure regulation and control.

Description

technical field [0001] The invention relates to the technical field of copolymers, in particular to a polysiloxane functionalized ethylene-norbornene copolymer and a preparation method thereof. Background technique [0002] Ethylene-norbornene copolymer is a kind of copolymer with novel structure and properties. Different from traditional polyolefins, the cycloalkane structure is introduced into the main chain of cycloolefin copolymer, which also endows it with excellent transparency, chemical stability, heat resistance and refractive index. It is used in optical parts, electronic components, Fields such as medical devices and packaging show great potential. In order to further broaden its application range, introducing polar groups to functionalize it is an important method. However, for the direct copolymerization of functionalized norbornene and ethylene to prepare functionalized ethylene-norbornene copolymers, the selection of catalysts in related studies is mostly lim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/12C08F210/02
CPCC08F283/124C08F210/02
Inventor 范宏田保政蔡育铨
Owner ZHEJIANG UNIV