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Preparation method of block polymer with adjustable molecular weight distribution

A molecular weight distribution and block polymer technology, applied in the field of block polymer preparation, can solve the problems of high polymerization reaction temperature, inability to adjust product molecular weight distribution, harsh reaction conditions, etc.

Active Publication Date: 2022-04-01
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] CN 110128577 A discloses a method for the polymerization of methacrylate monomers regulated by near-infrared light, and CN110128578A discloses a method for the reversible inactivation free radical polymerization of water-soluble monomers in aqueous solution induced by iodine and polymer nanoparticles The preparation method and the polymerization process all have the characteristics of "living" free radical polymerization, but the distribution of the obtained polymers is relatively narrow, and the molecular weight distribution of the product cannot be adjusted in a wide range
Literature Angew.Chem.2019, 131, 5654–5659 reported a method to control the degree of polymerization by utilizing temperature-selective free radical generation in organocatalyzed living radical polymerization, using MMA and BA copolymerization, although the method The molecular weight distribution of the product can be regulated, but the polymerization reaction temperature used in this method is relatively high (70-110°C), the reaction conditions are relatively harsh, and the energy consumption is relatively high, which is not conducive to practical application

Method used

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  • Preparation method of block polymer with adjustable molecular weight distribution
  • Preparation method of block polymer with adjustable molecular weight distribution
  • Preparation method of block polymer with adjustable molecular weight distribution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In this implementation, the polymerization kinetics of MMA in DMI solvent was studied without adding an end-capping agent. Polymerization was carried out in 5 mL ampoules under argon atmosphere. The light source is a blue light-emitting diode (LED) lighting device (λ max =460nm, 18.6mW / cm 2 ). Initial feed molar ratio [MMA] 0 / [n-BA] 0 / [CP-I] 0 = 100 / 0 / 1. Add MMA, CP-I (0.047mmol), DMI and a clean magnetic stirrer to a clean 5mL ampoule respectively. After at least three freeze-pump-fill-thaw cycles to de-oxygenize the vial and provide an argon (Ar) atmosphere, the ampoule is promptly flame-sealed. Subsequently, the ampoule was placed in a magnetic stirrer with a blue LED lighting device installed in advance, and the distance between the ampoule and the light source was about 1.5 cm. The heat generated by the light source and the polymerization system was removed by circulating cooling in a constant temperature water bath, and the polymerization reaction was al...

Embodiment 2

[0049] In this embodiment, MMA is used as the first polymerizable monomer, n-BA is used as the end-capping agent, and CP-I is used as the initiator, and MMA is photopolymerized in DMI at room temperature, and the polymerization reaction is carried out in a 5mL ampoule in neutral and argon atmosphere. The light source is a blue light-emitting diode (LED) lighting device (λ max =460nm, 18.6mW / cm 2 ). change [MMA] 0 / [n-BA] 0 / [CP-I] 0 different molar ratios to prepare different PMMA. Among them, [MMA] 0 / [n-BA] 0 / [CP-I] 0 See Table 1 for the molar ratios.

[0050] In the initial molar ratio [MMA] 0 / [n-BA] 0 / [CP-I] 0 The polymerization reaction of =90 / 10 / 1 is an example: add MMA (4.24mmol), n-BA (0.47mmol), CP-I (0.047mmol), DMI (0.5mL) and a A clean magnetic stir bar. After at least three freeze-pump-fill-thaw cycles to de-oxygenize the vial and provide an argon (Ar) atmosphere, the ampoule is promptly flame-sealed. Subsequently, the ampoule was placed in a mag...

Embodiment 3

[0056] Prepare PMMA according to the method for embodiment 2, molar ratio [MMA] 0 / [n-BA] 0 / [CP-I] 0 =90 / 10 / 1, the difference is that the polymerization time distribution is 3, 6, 9, 12, 15, 20h, the results of the kinetic experiment are as shown in table 3, the polymer molecular weight distribution can be adjusted under this ratio The range is between 1.28-1.53.

[0057]Polymerization kinetics under the fixed ratio of MMA and n-BA in table 3

[0058]

[0059] In Table 3, R=[MMA] 0 / [n-BA] 0 / [CP-I] 0 ,V MMA =0.45mL,V DMI = 0.5 mL. Conv. (conversion ratio) was determined gravimetrically. m n,th by [MMA] 0 ,[n-BA] 0 ,[CP-I] 0 and the monomer conversion rate was calculated. m n,GPC Represents the molecular weight measured by GPC; M w / M n Represents molecular weight distribution index, which is obtained by GPC test.

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Abstract

The present invention relates to a method for preparing a block polymer with adjustable molecular weight distribution. The preparation method includes the following steps: using methacrylate monomers as first polymerization monomers, using acrylate monomers as end capping agents, using iodine compounds as initiators, and using methacrylate monomers as first polymerization monomers in DMI Photopolymerization occurs, and after the reaction is complete, polymethacrylate terminated with acrylate monomer is obtained; the polymethacrylate terminated with acrylate monomer is used as a macroinitiator, and the acrylate monomer is used as the second polymerization Monomer, using copper as catalyst and amine compound or bipyridine as ligand, the second polymerized monomer is polymerized in DMI, and the block copolymer of polymethacrylate and polyacrylate is obtained after the reaction is complete . The present invention provides a method for regulating the molecular weight distribution of the block polymer under the premise of maintaining the "activity" of the block polymer.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a preparation method of a block polymer with adjustable molecular weight distribution. Background technique [0002] Reversible-deactivation radical polymerization (RDRP) is relatively mature in the research of polymer molecular weight and molecular weight distribution control, structure design and synthesis, etc. material has unique advantages. Complex polymer structures are often accompanied by unique properties, and the synthesis of polymers with different topological structures has promoted the application of corresponding polymer materials in various fields. Polymer Molecular Weight Distribution Index The glass transition temperature of the polymer (T g ), mechanical properties, rheological properties and other physical properties are significantly affected, and the properties of polymer materials with different molecular weight distribution indices or the same...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00
CPCC08F293/005C08F2438/03
Inventor 程振平倪媛媛张丽芬朱秀林
Owner SUZHOU UNIV