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A Living Polymerization System Based on Phosphine-Based Catalyzed Synthesis of Ultra-High Molecular Weight Polymers

An ultra-high molecular weight, base-catalyzed technology, applied in the field of polymer synthesis, can solve the problems of large amount of catalyst, harsh reaction conditions, and wide molecular weight distribution of polymers, etc., to achieve wide applicability of substrates, mild reaction conditions, and narrow molecular weight distribution Effect

Active Publication Date: 2020-12-11
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the bottleneck faced by the catalytic system for the synthesis of ultra-high molecular weight polymers is that the following problems cannot be solved at the same time: 1) the reaction conditions are harsh and difficult to operate; 2) the molecular weight distribution of the obtained polymer is wide; 3) transition metal catalysis is often required; 3) the reaction Slow, uncontrollable reaction, large difference between theoretical molecular weight and actual molecular weight; 4) Low initiation efficiency, large amount of catalyst; 5) Copolymerization between different monomers (random copolymerization and block copolymerization) cannot be carried out

Method used

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  • A Living Polymerization System Based on Phosphine-Based Catalyzed Synthesis of Ultra-High Molecular Weight Polymers
  • A Living Polymerization System Based on Phosphine-Based Catalyzed Synthesis of Ultra-High Molecular Weight Polymers
  • A Living Polymerization System Based on Phosphine-Based Catalyzed Synthesis of Ultra-High Molecular Weight Polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The conjugate addition polymerization of embodiment 1 methyl methacrylate (MMA)

[0041] There are three feeding methods in the polymerization process: 1. Pre-mix Lewis acid and Lewis base for 10 minutes, and then add monomer; 2. Pre-mix Lewis acid and monomer, and then add Lewis base; 3. Pre-mix Lewis base and monomer, and then Add Lewis acid. Regardless of the feeding method, the polymerization of methyl methacrylate can be well achieved.

[0042] The polymerization reaction was carried out in a glove box, and methyl methacrylate (0.5mL, 4.68mmol) and toluene were measured and placed in a 20ml reaction bottle (the total volume of the solution obtained was 5mL), and Lewis base and Lewis acid were added respectively, and started Timing and stirring for a period of time until the monomers are completely converted, the reaction bottle is taken out of the glove box, and 5% HCl / methanol solution is added to terminate the polymerization reaction. The polymer was filtered o...

Embodiment 2

[0047] The chain extension of embodiment 2MMA

[0048] The polymerization reaction was carried out in a glove box, and a certain amount of (BHT)Al was weighed i Bu 2 In the 20 milliliter reaction bottle, add MMA (0.5ml, 4.7mmol), after treating that monomer and Lewis acid fully react, add dichloromethane as solvent (solution total volume is 5mL), add the IAP3 that has weighed, and Start timing, stir until the monomers are completely converted, then add the same amount of MMA (0.5ml, 4.7mmol), repeat this several times, after all the monomers are completely converted, take the reaction bottle out of the glove box, add 5 % HCl / methanol solution to terminate the polymerization. The polymer was filtered off, washed thoroughly with methanol, and dried under vacuum at 50°C to constant weight. The molecular weight and molecular weight distribution of the resulting polymers were determined by gel permeation chromatography.

[0049] Using IAP3 with (BHT)Al i Bu 2 The results of c...

Embodiment 3

[0052] Copolymerization of embodiment 3 methyl methacrylate (MMA) and ethyl methacrylate (EMA)

[0053] Taking the preparation of poly(PMMA-block-PEMA-block-PMMA) as an example: the polymerization reaction is carried out in a glove box, and a certain amount of Lewis acid is weighed in a 20 ml reaction bottle, and MMA (0.5ml, 4.7mmol) is added After the monomer and Lewis acid fully reacted, add tetrahydrofuran as a solvent (the total volume of the solution is 5mL), add the weighed IAP3, and start timing, stir for a period of time, and then add EMA (632 μL , 4.7mmol), after the complete conversion of the monomers, add MMA (0.5ml, 4.7mmol), after the complete conversion of all the monomers, take the reaction bottle out from the glove box, add 5% HCl / methanol solution to terminate the polymerization reaction . The polymer was filtered off, washed thoroughly with methanol, and dried under vacuum at 50°C to constant weight. The molecular weight and molecular weight distribution of...

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Abstract

The invention provides an active polymerization system based on synthesis of ultrahigh molecular weight polymer catalyzed by phosphine alkali, which belongs to the technical field of polymer synthesis. In an organic solvent, a vinyl polar monomer is used as a monomer raw material, and conjugate addition polymerization is performed under synergic catalysis of Lewis acid and Lewis base, wherein theLewis base is a phosphine compound. The active polymerization system based on synthesis of ultrahigh molecular weight polymer catalyzed by phosphine alkali has the advantages of easy raw material obtaining, convenient operation, mild reaction conditions, high speed, high conversion rate, wide monomer adaptability, small catalyst usage amount, controllable molecular weight of polymers, narrow molecular weight distribution, and activity-controlled polymerization, and copolymerization between monomers of different polarities can be realized.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to an active polymerization system for synthesizing ultrahigh molecular weight polymers based on phosphine base catalysis. Background technique [0002] Polymethyl methacrylate, PMMA, commonly known as plexiglass. PMMA has many excellent properties and has been widely used in aviation, construction, agriculture, optical instruments and other fields. However, the long-term use temperature of PMMA is low (under 65°C), the heat resistance is not high, the surface hardness is low, and the disadvantages such as high hygroscopicity limit its application range. People have been trying to improve some of its properties and expand its application fields. The molecular weight of high molecular polymer is one of the most important indicators of product quality. PMMA with molecular weight higher than 1 million is usually called ultra-high molecular weight PMMA. It has b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F4/54C08F297/02C08F220/14C08F220/18
CPCC08F4/54C08F120/14C08F220/14C08F220/18C08F297/026
Inventor 张越涛何江华白云
Owner JILIN UNIV
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