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Method for preparing regioblock copolymers of isoprene and myrcene by chain transfer reaction

A technology of isoprene and myrcene, which is applied in the field of catalyzing the polymerization of isoprene or myrcene to form di- or multi-block regional copolymers, which can solve the disadvantages of environmental protection and energy saving, and no report on isoprene regional copolymers , increase production costs and other issues

Active Publication Date: 2016-08-24
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process, a large amount of solvent and energy are used to complete mixing, drying, etc., which is not conducive to environmental protection and energy saving requirements, and also increases production costs.
So far, although Cai Zhengguo and others have synthesized multi-block domain copolymers of butadiene (references: Z. Cai, M. Shinzawa, Y. Nakayama, T. Shiono. Macromolecules 2009, 42, 7642-7643), but have not yet See reports on isoprene domain copolymers, especially reports on the synthesis of di- or multi-block domain copolymers with controllable block length and composition

Method used

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  • Method for preparing regioblock copolymers of isoprene and myrcene by chain transfer reaction
  • Method for preparing regioblock copolymers of isoprene and myrcene by chain transfer reaction
  • Method for preparing regioblock copolymers of isoprene and myrcene by chain transfer reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Weigh 0.0155 g (0.01 mmol) of complex 1a into a 100 mL eggplant-shaped bottle, dissolve it with 18 mL of chlorobenzene, then weigh 0.511 g (7.5 mmol) of isoprene, and inject 100 μL of 1M Al i Bu 3 The n-hexane solution was injected into the above mixture. Weigh 0.0185 g (0.02 mmol) [Ph3C][B(C6F5)4] (cocatalyst borate), add 2mL of chlorobenzene to dissolve, and transfer to the dropping funnel. Assemble the dropping funnel and the eggplant-shaped bottle, start stirring, and quickly add the co-catalyst into the solution after constant temperature at 25 degrees Celsius. After 10 min, add 100 μL of 1 M AlMe 3 The n-heptane solution was stirred for 2 minutes, then 0.511 g (7.5 mmol) of isoprene was added and reacted for 45 minutes. After the reaction, ethanol was slowly added dropwise with stirring until the solid was completely precipitated. The liquid was decanted and the 3,4 and 1,4-polyisoprene copolymers were obtained as white solids. Dry in a vacuum oven at 60°C t...

Embodiment 2

[0048] Weigh 0.0156 g (0.01 mmol) of complex 1b into a 100 mL eggplant-shaped bottle, dissolve it with 18 mL of chlorobenzene, then weigh 0.511 g (7.5 mmol) of isoprene, add 100 μL of 1M Al i Bu 3 The n-hexane solution was injected into the above mixture. Weigh 0.0185 g (0.02 mmol) [Ph3C][B(C6F5)4] (cocatalyst borate), add 2mL of chlorobenzene to dissolve, and transfer to the dropping funnel. Assemble the dropping funnel and the eggplant-shaped bottle, start stirring, and quickly add the co-catalyst into the solution after constant temperature at 25 degrees Celsius. After 10 min, add 100 μL of 1 M AlMe 3 The n-heptane solution was stirred for 2 minutes, then 0.511 g (7.5 mmol) of isoprene was added and reacted for 45 minutes. After the reaction, ethanol was slowly added dropwise with stirring until the solid was completely precipitated. The liquid was decanted and the 3,4 and 1,4-polyisoprene copolymers were obtained as white solids. Drying in a vacuum oven at 60°C until...

Embodiment 3

[0050] Weigh 0.0156 g (0.01 mmol) of complex 1b into a 100 mL eggplant-shaped flask, dissolve it with 18 mL of chlorobenzene, then weigh 0.511 g (7.5 mmol) of isoprene, add 100 μL of Al i Bu 3 The n-hexane solution was injected into the above mixture. Weigh 0.0185 g (0.02 mmol) [Ph3C][B(C6F5)4] (cocatalyst borate), add 2 mL of chlorobenzene to dissolve, and transfer to the dropping funnel. Assemble the dropping funnel and the eggplant-shaped bottle, start stirring, and quickly add the co-catalyst into the solution after constant temperature at 25 degrees Celsius. After 10 min, add 140 μL of 1M AlMe 3 The n-heptane solution was stirred for 2 minutes, then 0.511 g (7.5 mmol) of isoprene was added and reacted for 45 minutes. After the reaction, ethanol was slowly added dropwise with stirring until the solid was completely precipitated. The liquid was decanted and the 3,4 and 1,4-polyisoprene copolymers were obtained as white solids. After drying in a vacuum oven at 60°C to ...

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Abstract

The invention belongs to the technical field of conjugated olefin polymerization, in particular to a method for preparing isoprene and myrcene regional block copolymers through chain transfer reactions. The invention utilizes a rare earth / organoboron salt catalyst system to catalyze isoprene and myrcene for solution polymerization, and only uses one monomer to obtain 3,4 and 1,4-polyconjugated by adding two different alkylaluminum reagents Olefin regional copolymers, or the use of two or more monomers, to obtain three or four block or multi-block copolymers. The conversion rate of monomer can reach 100%. The block length and composition of the products are highly controllable. In the copolymer, the content of 3,4-product is usually controlled between 10%-90%, the molecular weight of the product is between 60000-125000, and the molecular weight distribution is between 1.4-1.8. All domain copolymers obtained by this method are reported for the first time; by changing the type and amount of added monomers, polymer materials with different structures and compositions can be obtained, which has broad application prospects.

Description

technical field [0001] The invention belongs to the technical field of conjugated olefin polymerization, and in particular relates to a method capable of catalyzing the polymerization of isoprene or myrcene to generate di- or multi-block domain copolymers. Background technique [0002] Polyolefins, as an important class of polymer materials, have greatly improved the living environment and living conditions of human beings. Correspondingly, the polyolefin industry has also become a pillar industry of the national economy and an important symbol of the development of a country's petrochemical industry. Among various polyolefin materials, polyconjugated olefin is a polymer with many excellent properties and broad application prospects. Many of them are high-performance rubber or plastic. Among them, polyisoprene (IR), which can be artificially synthesized in large quantities, can be divided into cis-1,4-IR, trans-1,4-IR and 3,4-IR. The cis-1,4-IR is the main natural rubber ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/08C08F136/22C08F297/06C08F4/52
Inventor 张立新郁夏盈
Owner FUDAN UNIV
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