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Method for preparing functionalized polyolefin by continuous flow polymerization-polymerization coupling

A polyolefin and functionalization technology, which is used in the field of continuous flow polymerization-polymerization coupling to prepare functionalized polyolefins, can solve the problems of low conversion efficiency of active centers, cumbersome process routes, harsh reaction conditions, etc., and avoid switching and cumbersome operations. Steps, avoid oxidative inactivation, meet the effect of isolation conditions

Active Publication Date: 2019-02-01
NANJING UNIV OF TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a method for preparing functionalized polyolefins through continuous flow polymerization-polymerization coupling to solve the problems in the prior art such as cumbersome process routes, low conversion efficiency of active centers, and low reaction efficiency. Issues such as harsh conditions and long reaction times

Method used

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  • Method for preparing functionalized polyolefin by continuous flow polymerization-polymerization coupling
  • Method for preparing functionalized polyolefin by continuous flow polymerization-polymerization coupling
  • Method for preparing functionalized polyolefin by continuous flow polymerization-polymerization coupling

Examples

Experimental program
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Effect test

Embodiment 1

[0035](1) Anionic polymerization: Take purified styrene (7.2mL, 63mmol) in the glove box and dissolve it in 22.8mL cyclohexane, and the 1-1 solution (2.1mol / L, 135eq) is prepared; take sec-butyllithium (1mL, 1.3mmol) was dissolved in 29mL cyclohexane, and the 1-2 solution (0.047mol / L, 3eq) was configured; the 1-1 solution and 1-2 solution were used at the same flow rate (0.04 mL / min) into T-type mixer M1 and tubular reactor R1. The tubular reactor was placed in a magnetic stirrer to control the temperature, the reaction temperature was controlled at 0°C and 25°C respectively, the residence time of the reaction was 25min, and the A solution was obtained from the reaction.

[0036] (2) Synthesis of macromolecular borane initiator: take BF in the glove box 3 OEt 2 The solution (0.7mL, 0.48mmol) was dissolved in 29.4mL cyclohexane, and the 2-1 solution (0.016mol / L, 1eq) was prepared; the 2-1 solution was reacted with the A solution obtained in step (1) at the same flow rate (16...

Embodiment 2

[0044] (1) Anionic polymerization: prepare respectively cyclohexane solution 1-1 (1.41mol / L, 90eq; 2.10mol / L, 135eq; 2.82mol / L, 180eq) of styrene in the glove box; take sec-butyllithium ( 1mL, 1.3mmol) was dissolved in 29mL cyclohexane, and the 1-2 solution (0.047mol / L, 3eq) was prepared; the 1-1 solution and 1-2 solution were used at the same flow rate (0.04mL / min) into the T-type mixer M1 and the tubular reactor R1. The tubular reactor was placed in a magnetic stirrer to control the temperature, the reaction temperature was controlled at 25° C., the residence time of the reaction was 25 min, and A solution was obtained from the reaction.

[0045] (2) Synthesis of macromolecular borane initiator: take BF in the glove box 3 OEt 2 The solution (0.7mL, 0.48mmol) was dissolved in 29.4mL cyclohexane, and the 2-1 solution (0.016mol / L, 1eq) was prepared; the 2-1 solution was reacted with the A solution obtained in step (1) at the same flow rate (16 μL / min) into the T-type mixer ...

Embodiment 3

[0053] (1) Anionic polymerization: prepare cyclohexane solutions 1-1 (2.1mol / L, 135eq) of styrene, butadiene, isobutylene or methyl methacrylate in the glove box; take sec-butyllithium (1mL, 1.3mmol) was dissolved in 29mL cyclohexane, and the 1-2 solution (0.047mol / L, 3eq) was prepared; the 1-1 solution and 1-2 solution were used at the same flow rate (0.04mL / min ) into the T-type mixer M1 and the tubular reactor R1. The tubular reactor was placed in a magnetic stirrer to control the temperature, the reaction temperature was controlled at 25° C., the residence time of the reaction was 25 min, and A solution was obtained from the reaction.

[0054] (2) Synthesis of macromolecular borane initiator: take BF in the glove box 3 OEt 2 The solution (0.7mL, 0.48mmol) was dissolved in 29.4mL cyclohexane, and the 2-1 solution (0.016mol / L, 1eq) was prepared; the 2-1 solution was reacted with the A solution obtained in step (1) at the same flow rate (16 μL / min) into the T-type mixer M2...

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Abstract

The invention discloses a method for preparing functionalized polyolefin by continuous flow polymerization-polymerization coupling. The method comprises the following steps: respectively dissolving amonomer and an initiator in a first organic solvent in an inert gas atmosphere, respectively simultaneously pumping the obtained two solutions into a first micromixer in a microreactor, and fully reacting the two solutions in the first microreactor to obtain a solution A; dissolving an organoboron reagent in a second organic solvent in the inert gas atmosphere, mixing the obtained organoboron solution with the solution A in a second micromixer, and carrying out a sufficient reaction in the second microreactor to obtain a solution B; reacting NaH with trimethyl sulfoxide in toluene under the protection of an inert gas to obtain a monomer Ylide solution, mixing the monomer Ylide solution with the solution B in a third micromixer, performing a sufficient reaction in the third microreactor, and collecting the obtained reaction solution C; and oxidizing, filtering, washing and drying the collected reaction solution C to obtain the functionalized polyolefin.

Description

technical field [0001] The invention relates to a method for preparing functionalized polyolefin through continuous flow polymerization-polymerization coupling, which belongs to the field of polymer synthesis. Background technique [0002] Polyolefin is a general-purpose thermoplastic polymer material with wide application and low price, and plays an important role in daily life and national economy. However, the intrinsic structure of polyolefins leads to limitations in its performance and applications. For example, the molecular weight distribution index is generally wide, the polarity is low, and the compatibility and adhesion with other materials are poor, which restricts the performance of polyolefin materials. Further improvement and expansion of application fields. [0003] The traditional synthesis routes of functionalized polyolefins are all based on the addition of π bonds, including coordination polymerization, chain transfer and group functionalization. These s...

Claims

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Application Information

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IPC IPC(8): C08F297/02C08F297/04C08F8/06
CPCC08F8/06C08F297/02C08F297/048
Inventor 郭凯赵婉茹朱宁胡欣方正王剑陈柯睿
Owner NANJING UNIV OF TECH
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