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A continuous flow polymerization-polymerization coupling method for preparing functionalized polyolefins

A polyolefin and functionalization technology, which is applied in the field of continuous flow polymerization-polymerization coupling to prepare functionalized polyolefins, can solve the problems of low conversion efficiency of active centers, harsh reaction conditions, cumbersome process routes, etc., avoiding operation steps and improving transmission efficiency. quality, avoid the effect of oxidative inactivation

Active Publication Date: 2022-04-29
NANJING TECH UNIV
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  • Abstract
  • 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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  • A continuous flow polymerization-polymerization coupling method for preparing functionalized polyolefins
  • A continuous flow polymerization-polymerization coupling method for preparing functionalized polyolefins
  • A continuous flow polymerization-polymerization coupling method for preparing functionalized polyolefins

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. In an inert gas atmosphere, monomers and initiators are respectively dissolved in a first organic solvent, and then the two solutions are simultaneously pumped into the micro-reaction Mix in the first micro-mixer in the device, and fully react in the first micro-reactor to obtain solution A; in an inert gas atmosphere, dissolve the organic boron reagent in the second organic solvent, and then mix the organic boron solution with The obtained solution A was mixed in the second micro-mixer, fully reacted in the second micro-reactor to obtain solution B; under the protection of an inert gas, NaH and trimethylthionyl chloride were reacted in toluene to obtain mono ylide solution, then mix it with the obtained solution B in the third micro-mixer, fully react in the third micro-reactor, and collect the reaction solution C; the final collected reaction solution C is oxidized, filtered, washed, and dried Get it later.

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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Patent Type & Authority Patents(China)
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 TECH UNIV
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