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A kind of preparation method of alkoxysilane-olefin copolymer and its product and application

A technology of alkoxysilane and olefin copolymer, which is applied in the field of polyolefin functional modification, can solve the problems of difficult preparation of metallocene catalysts, low reactivity, and unsatisfactory copolymerization effect, etc., and achieve excellent crosslinking performance and reactivity High, easy-to-structure effect

Active Publication Date: 2019-02-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there have been related reports on the use of metallocene catalysts to copolymerize alkoxysilanes and olefins (ZIMMER, S.SCH BEL, A.HALBACH, T, et al., New Curable Propylene Copolymers Containing Tert-Butoxysilane Side Groups. Macromolecular Rapid Communications 2013,34(3),221-226.), but because metallocene catalysts are difficult to prepare, they are sensitive to polar monomers, resulting in low reactivity, and the cocatalyst MAO or MMAO used is easy to cause condensation during the copolymerization process. Glue, so the copolymerization effect is not ideal
It can be seen that it is still very challenging to select a suitable catalytic system to realize the coordination copolymerization of olefins and alkoxysilanes.

Method used

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  • A kind of preparation method of alkoxysilane-olefin copolymer and its product and application
  • A kind of preparation method of alkoxysilane-olefin copolymer and its product and application
  • A kind of preparation method of alkoxysilane-olefin copolymer and its product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) In a 250mL three-necked flask, add 16.5g (150mmol) 1,7-octadiene, 30g toluene and 0.067g (30ppm) Karstedt catalyst solution (the mass concentration of platinum is 2%), and pass into the reaction system After nitrogen protection and stirring, 3.1 g (30 mmol) of dimethylethoxysilane was slowly added dropwise, and the reaction was continued at 40° C. for 8 hours after the dropwise addition was completed. After the reaction, the crude product is rotary evaporated to remove unreacted raw materials, and the catalyst is removed by passing through a silica gel column to obtain a clear and transparent oily liquid that is double bond-terminated alkoxysilane. It can be seen from the characterization of the hydrogen NMR spectrum that in the double bond-terminated alkoxysilane, a=4 and the purity is 98%.

[0044] (2) Fully dry the 250mL three-neck flask equipped with a mechanical stirring paddle to remove water and oxygen, continuously fill the system with ethylene gas and keep ...

Embodiment 2

[0048] Repeat the steps of Example 1, except that the amount of double bond-terminated alkoxysilane added in step (2) is 0.43g (20mmol / L), and the calculated reactivity is 5.8kg·mmol V -1 h -1 . The copolymerized product was confirmed to be a copolymer with alkoxysilane branch and olefin main chain by H NMR spectrum and infrared spectrum. It can be seen from the high temperature nuclear magnetic spectrum analysis that the molar content of the alkoxysilane component in the copolymer is 0.55%. As determined by high-temperature GPC analysis, the weight-average molecular weight of the copolymer is 29.7kg / mol, the PDI is 3.6, and the gel content of the product reaches 86% after crosslinking.

Embodiment 3

[0050] The procedure of Example 1 was repeated except that the monohydroterminated alkoxysilane added in step (1) was methyldiethoxysilane (4.0 g, 30 mmol). The product of step (1) is double bond-terminated alkoxysilane. It can be seen from the characterization of the hydrogen NMR spectrum that in the double bond-terminated alkoxysilane, a=4 and the purity is 98%.

[0051] In step (2), the amount of double bond-terminated alkoxysilane becomes 0.73g (30mmol / L), and the calculated reactivity is 3.8kg·mmol V -1 h -1 . The copolymerized product was confirmed to be a copolymer with alkoxysilane branch and olefin main chain by H NMR spectrum and infrared spectrum.

[0052] According to nuclear magnetic analysis, the molar content of the alkoxysilane component in the copolymer is 0.62%. According to high-temperature GPC analysis, the weight-average molecular weight of the copolymer is 18.4kg / mol, the PDI is 2.0, and the gel content of the product after crosslinking reaches 99%. ...

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Abstract

The invention relates to a preparation method of an alkoxy silane-olefin copolymer. The preparation method comprises the following steps: firstly, carrying out hydrosilylation reaction on single hydrogen-terminated alkoxy silane and straight chain alpha, omega-diene under the action of a platinum catalyst to generate double bond-terminated alkoxy silane; secondly, carrying out coordinated copolymerization reaction on the double bond-terminated alkoxy silane and alpha-olefin under the action of a Ziegler-Natta vanadium-based main catalyst and a diethylaluminium chloride Et2AlCl cocatalyst system to generate the alkoxy silane-olefin copolymer. The invention also relates to a product obtained by the preparation method and application. By improving the method, the gel phenomenon is not caused during preparation of the alkoxy silane-olefin copolymer; in addition, the obtained product can be quickly crosslinked in an acidic environment; the content of the crosslinked gel reaches 10 to 100 percent, thereby realizing functional modification of a polyolefin material.

Description

technical field [0001] The invention relates to the field of polyolefin functional modification, in particular to a preparation method of an alkoxysilane-olefin copolymer and its product and application. Background technique [0002] Silicone materials usually contain Si-O bonds with high bond energy, in which Si atoms are connected to other organic groups, and the special structure endows them with excellent properties, such as crosslinkability, low surface energy, weather resistance, thermal stability etc. It can be used as cross-linking materials, processing modifiers, surface modifiers, flame retardants, etc., and has broad application prospects. However, its poor mechanical properties and incompatibility with carbon-based materials affect the overall performance of the material, thereby limiting its application range. [0003] Based on the advantages of light weight, low cost and strong replaceability, polyolefins are widely used in modern industry and social life. Ho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/02C08F230/08C08F4/68C08J3/24C08L23/08
CPCC08F210/02C08J3/24C08J2323/08C08F230/08C08F4/68
Inventor 范宏刘智颖金震
Owner ZHEJIANG UNIV
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