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Oxygen-mediated free radical polymerization method

A free radical-mediated technology, applied in the field of polymers, to achieve good catalytic performance, low energy consumption, and strong stability

Pending Publication Date: 2022-05-17
FUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Developing efficient and stable heterogeneous photocatalysts is an ideal way to solve this problem, however, finding sustainable and stable heterogeneous photocatalysts to catalyze oxygen-mediated light-induced CRP remains a challenge.

Method used

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  • Oxygen-mediated free radical polymerization method
  • Oxygen-mediated free radical polymerization method
  • Oxygen-mediated free radical polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) 4,4',4'',4'''-(porphyrin-5,10,15,20-tetra)aniline (H 2 -TCPP) synthesis: Add 4-nitrobenzaldehyde (22.0 g, 145 mmol), propionic acid (600 mL) and acetic anhydride (24 mL) into a 1000-mL flask under N 2 middle reflux. Subsequently, pyrrole (10 mL) was added via syringe, and the mixture was reacted for 12 h. After the mixture was cooled to room temperature, it was placed in the refrigerator overnight, and the solid was filtered, washed with distilled water (200 mL) and methanol (500 mL), and dried in vacuo. Subsequently, the solid was dissolved in pyridine (160 mL) with N 2 Refluxed for 12 h under protection, the mixture was cooled to room temperature, filtered to obtain a black solid, washed with acetone to obtain a purple solid. The product and SnCl 2 2H 2 O (18.0 g, 7.97 mmol) was added to hot concentrated hydrochloric acid (500 mL) solution, N 2 Reflux overnight under atmosphere. The mixture was cooled to 0 °C with ice water and neutralized to pH = 8 with co...

Embodiment 2

[0048] Get embodiment 1 product (1) H 2 -TCPP-DHTA-COFs 1 mg, MMA (2 mL, 18.6 mmol), CPADB (26 mg, 0.093 mmol), TEA (134 μL, 0.93 mmol) and DMAC (1 mL) were added to a 4 mL glass bottle, and the stopper was closed Rubber stopper, with white LED strip (13W m -1 , 15mW cm -2 ) irradiation. Take a small amount of the mixture at a pre-designed time, and use gel permeation chromatography (GPC) to measure the conversion rate and molecular weight M n and molecular weight distribution M w / M n and other parameters.

[0049] image 3 A schematic diagram of the polymerization process; Figure 4 is the molecular weight M n ,The molecular weight distribution M w / M n Relational figure with conversion rate and the outflow curve figure of the polymer product measured by GPC; Figure 5 for ln( M 0 / M t ) Polymerization kinetics curve as a function of time t, where M 0 is the initial monomer concentration, M t is the monomer concentration at time t, it can be seen ...

Embodiment 3

[0052] Take the product of Example 1 (2) Zn-TCPP-DHTA-COFs 1 mg, MMA (2 mL, 18.6 mmol), CPADB (26 mg, 0.093 mmol), TEA (134 μL, 0.93 mmol) and DMAC (1 mL) were added 4 mL glass vial with a rubber stopper and a white LED strip (13W m -1 , 15mW cm -2 ) irradiation. Take a small amount of the mixture at a pre-designed time, and use gel permeation chromatography (GPC) to measure the conversion rate and molecular weight M n and molecular weight distribution M w / M n and other parameters.

[0053] Image 6 is the molecular weight M n ,The molecular weight distribution M w / M n Graph vs. conversion rate, Figure 7 It is a polymerization kinetic curve, and the combination of the two shows that a polymer with controllable molecular weight and narrow molecular weight distribution can be obtained under this polymerization condition.

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Abstract

The invention discloses an oxygen-mediated free radical polymerization method, which is characterized in that a porphyrinyl covalent organic framework (COFs) material is used as a catalyst, amine is used as a promoter, and reversible addition-fragmentation chain transfer (RAFT) polymerization is carried out under oxygen mediation to prepare a polymer with accurate molecular weight and narrow molecular weight distribution. Meanwhile, the porphyrin-based covalent organic framework material used in the method is high in stability, high in catalytic efficiency and excellent in cycle performance, and is an ideal platform for constructing a photoinduced RAFT polymerization efficient heterogeneous catalyst under the aerobic condition.

Description

technical field [0001] The invention belongs to the field of macromolecules, and more specifically relates to a method for oxygen-mediated controllable radical polymerization. Background technique [0002] Controlled radical polymerization (CRP) technology has attracted much attention for the preparation of structurally precise and fully functional polymers and advanced materials. In the past few decades, the development of CRP technology has achieved some revolutionary innovations, such as atom transfer radical polymerization (ATRP), reversible addition-fragmentation chain transfer (RAFT) polymerization, nitroxide-mediated polymerization (NMP ), reversible complexation-mediated polymerization (RCMP), etc. Among them, the RAFT polymerization monomer has strong universality, is very beneficial to the polymerization reaction of vinyl monomers containing special functional groups, and has broad industrial application prospects. The reaction conditions of photopolymerization t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F120/18C08F120/34C08F120/28C08F2/38C08F2/46C08F4/50C08G83/00
CPCC08F120/14C08F120/18C08F120/34C08F120/28C08F2/38C08F2/46C08F4/50C08G83/008C08F2438/03
Inventor 侯琳熙卢振付晓玲杨宏杰肖龙强
Owner FUZHOU UNIV
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