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Visible-radiation-based water-soluble monomer atom transfer radical polymerization (ATRP) method

A water-soluble monomer, atom transfer technology, applied in chemical recovery and other directions, can solve the problems of restricting the large-scale application of ATRP and restricting its application, and achieve the effects of reducing metal salt residues, efficient recovery, and high catalyst recovery efficiency.

Active Publication Date: 2016-05-25
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, most polymerizations need to go through strict and cumbersome oxygen removal steps; catalysts need to be reactivated in an inert atmosphere before they can be reused; almost all ATRP catalyst separation and recovery methods are only suitable for the polymerization of oil-soluble monomers, and very few Water-soluble monomers are seldom involved; most of the polymerizations are carried out at relatively high reaction temperatures, and there is little involvement in the recovery of catalysts at room temperature and under visible light conditions. These problems limit the large-scale application of ATRP, especially limit its application in the biological field

Method used

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  • Visible-radiation-based water-soluble monomer atom transfer radical polymerization (ATRP) method
  • Visible-radiation-based water-soluble monomer atom transfer radical polymerization (ATRP) method
  • Visible-radiation-based water-soluble monomer atom transfer radical polymerization (ATRP) method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1: A method for atom transfer radical polymerization of water-soluble monomers based on visible light radiation.

[0049] (1) Synthesis of catalyst / ligand complex MCc:

[0050] Water-soluble monomer mPEGMA 500 (1.0mL, 2.12mmol), initiator EBPA (10.26mg, 4.24×10 -2 mmol), catalyst Cu(DC) 2 (10.0mg, 2.12×10 -2 mmol), ligand POA-ran-P(MA-Ln) (75.7mg, 4.24×10 -2 mmol) and UV photoinitiator TPO (3.6mg, 2.12×10 -2 mmol) into a 20mL flask filled with n-heptane (4.0mL) in advance, then add absolute ethanol (3.0mL) to it, and use a high-pressure mercury with a power of 10kW under the condition of a temperature of 30°C and mechanical stirring After the lamp was irradiated for 10 h, water (0.4 mL) was added to the flask to induce the solution to separate, and the upper n-heptane phase was removed to obtain a n-heptane solution of the catalyst / ligand complex MCc. Store at 2°C until use.

[0051] (2) Polymer PmPEGMA 500 Synthesis:

[0052] Water-soluble monomer mPEG...

Embodiment 2

[0053] Example 2: Investigation of the applicability of different monomer / initiator molar ratios.

[0054] ATRP has the advantage that the molecular weight of the polymer can be designed. Therefore, according to the method described in Example 1, polymers with different molecular weights can be obtained by changing the ratio of the monomer to the initiator. The results are shown in Table 1.

[0055]

[0056] Polymerization conditions: [mPEGMA 500 ] 0 / [EBPA] 0 / [MCc] / [CQ] 0 / [TEA] 0 =100 / x / 1 / 0.5 / 1, V mPEGMA500 =0.5mL, V 正庚烷 =2.0mL, V 乙醇 =1.5mL, temperature=25°C, time=22h.

[0057] It can be seen from Table 1 that under various monomer / initiator ratios, good polymerization results can be obtained, the molecular weight distribution is narrow, the GPC molecular weight is close to the theoretical molecular weight, and the polymerization rate increases with the increase of the ratio. There is a tendency to slow down, and the polymerization system has strong applicabil...

Embodiment 3

[0058] Example 3: Investigation of the applicability of different types of water-soluble monomers.

[0059] In order to investigate the applicability of different monomers to the method recorded in Example 1, it is planned to use DMAEMA, DMAA and NIPAM three kinds of water-soluble monomers to carry out parallel control experiments to study its ATRP situation under the irradiation of white LED lamps. The results As shown in table 2.

[0060]

[0061] Aggregation conditions: V M =0.5mL, V 正庚烷 =2.0mL, V 乙醇 =1.5mL, temperature=25°C, time=22h.

[0062] It can be seen from Table 2 that four different water-soluble monomers are suitable for the n-heptane / ethanol two-phase ATRP system, but the polymerization control of methacrylate monomers is obviously better than that of acrylamide monomers.

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Abstract

The invention discloses a visible-radiation-based water-soluble monomer atom transfer radical polymerization (ATRP) method. Particularly, the method comprises the following steps: 1) preparing a catalyst / ligand complex solution; 2) carrying out ATRP in an n-heptane / ethanol mixed solvent; 3) after the polymerization finishes, adding water to induce the solution to be stratified, and carrying out treatment to obtain a polymer; and 4) adding a new monomer, an initiator and a two-component visible photoinitiator into the recovered catalyst / ligand complex to carry out the next polymerization. The ATRP reaction is carried out under the mild efficient visible radiation, thereby implementing superhigh monomer conversion rate (greater than 95%) within a wider wavelength range, and obtaining the high-controllability polymer. The method can recycle the catalyst, is simple to operate, and has the advantages of high designability, lower cost, time saving and labor saving.

Description

technical field [0001] The invention belongs to the technical field of catalytic polymerization, and specifically relates to an atom transfer free radical that is carried out in a liquid / liquid two-phase system at room temperature and irradiated with visible light, and efficiently recovers and recycles catalysts at an ultra-high conversion rate aggregation method. Background technique [0002] Atom transfer radical polymerization (ATRP) is a powerful "living" / controllable radical polymerization method, which has attracted great attention in academia and industry since it was proposed in the 1990s. Although ATRP can synthesize polymers with controllable molecular weight and narrow molecular weight distribution, it must use a large amount of transition metal salts as catalysts to regulate the growth process of polymerization, and there will inevitably be catalyst residues in the resulting polymers. Not only will it impart a certain color to the polymer, but it will also cause...

Claims

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Application Information

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IPC IPC(8): C08F120/28C08F120/34C08F120/54C08F2/48
CPCY02P20/584C08F120/28C08F2/48C08F120/34C08F120/54
Inventor 程振平姜孝武张丽芬朱秀林
Owner SUZHOU UNIV
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