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A method of atom transfer radical polymerization based on liquid/liquid two-phase catalytic system

A catalytic system and atom transfer technology, applied in the field of catalytic polymerization, can solve the problems of high cost, time-consuming and laborious, and large-scale application limitations, and achieve the effects of simple operation, reduced metal salt residue, and strong designability

Active Publication Date: 2016-10-19
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although different catalyst separation and recovery methods have their own advantages, they also have many defects and deficiencies.
For example, the vast majority of polymerizations are conventional ATRP, which requires strict and cumbersome oxygen removal steps, and the reuse of catalysts requires reactivation under an inert atmosphere. Almost all ATRP catalyst recovery methods use ligands (a few is the initiator) modification and post-modification, the cost is high and time-consuming and labor-intensive, these problems have limited the large-scale application of ATRP (see Y. Q. Shen, H. D. Tang, S. J. Ding, Prog. Polym. Sci. ,2004, 29: 1053–1078)

Method used

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  • A method of atom transfer radical polymerization based on liquid/liquid two-phase catalytic system
  • A method of atom transfer radical polymerization based on liquid/liquid two-phase catalytic system
  • A method of atom transfer radical polymerization based on liquid/liquid two-phase catalytic system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: MMA aggregation based on liquid / liquid -based two -phase catalytic system.

[0044] In N 单体 : n 引发剂 : n 催化剂 : n 配体 : n 还原剂 = 200: 1: 2: 2: 0.2 Initial Murbi, the single MMA (1.0 ml, 9.44 mmol), the induced agent EBRPA (8.25 μL, 0.0472 mmol), the reducing agent AIBN (1.55 mg, 9.44 × 10 10 -3 mmol) Add to 2 mL toluene, and catalyst CUBR 2 (21.2 mg, 0.0944 mmol), the ligand TPMA (27.4 mg, 0.0944 mmol) is added to 2 ml of pure water, and the two phases of water and organic solvents are mixed in the clean 10 ml amp bottle. You do not need to pass the oxygen removal operation.Tube.Then transfer the amaranth bottle to the set temperature (75 ° C) and the speed (1800 RPM) oil bath pot. After the given time (24 h), take it out and place it in the ice water to cool the layered, and thenThe upper layer is diluted with THF and poured into a large amount of methanol.

Embodiment 2

[0045] Example 2: MMA aggregation based on liquid / liquid -based two -phase catalytic system.

[0046] In N 单体 : n 引发剂 : n 催化剂 : n 配体 : n 还原剂 = 100: 1: 1: 1: 0.1 Initial Moore, the single MMA (0.5 ml, 4.72 mmol), the induction EBRPA (16.5 μL, 0.0944 mmol), the reducing agent AIBN (1.55 mg, 9.44 × 10 10 -3 mmol) Add to 1 mL toluene, and catalyst CUBR 2 (21.2 mg, 0.0944 mmol), the ligand TPMA (27.4 mg, 0.0944 mmol) is added to 3 ml of pure water, and the two phases of water and organic solvents are mixed in the clean 10 ml amp bottle. You do not need to pass the oxygen removal operation.Tube.Then transfer the amaranth bottle to the set temperature (90 ° C) and the speed (1600 RPM) oil bath pot. After the given time (30 h), take it out and place it in the ice water to cool the layered, and thenThe upper layer is diluted with THF and poured into a large amount of methanol.

Embodiment 3

[0047] Example 3: Different types of causes catalyzed the effects of ATRP on both phases of liquid / liquid.

[0048] For ATRP aggregation, especially the ATRP aggregation of oil -soluble monomers in the water phase, ATRP causes a very critical role. It can affect the efficiency, polymerization rate, and end functionalization of the polymer during the entire aggregation stage, etc.EssenceTo this end, we plan to use different causes of dictating agents such as 2-bromotoxylxate (EBIB), α-bromodybenzhenylene (EBRPA), 2-bromoopraceraceae(BPN), MPEG550-BR and other parallel preparation of a series of polymers to examine the effects of MMA aggregation under the catalytic system of liquid / liquid catalytic system for several conventional ATRP. The results are shown in Table 1 below.

[0049]

[0050] Polymerization: Except [MMA] 0 : [MPEG550-br] 0 = 100: 1, [mma] 0 : [Caused] 0 : [Cubr 2 ] 0 : [TPMA] 0 : [AIBN] 0 = 200: 1: 2: 2: 0.2, V MMA Intersection V 水 Intersection V 甲苯 = 1: 2: 2, t =...

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Abstract

The invention discloses an atom transfer radical polymerization method based on a liquid / liquid two-phase catalytic system. The method comprises the following steps: mixing monomers, initiators, catalysts, ligands and reducing agents respectively dissolved in water and an organic solvent; performing a polymerization reaction at 60-90°C and a rotation speed of 1500-2000 rpm for 12~ 60 hours; after the completion, separate the two phases, pour the organic phase into methanol to precipitate, filter with suction, and dry to obtain the desired polymer; add monomer, initiator and reducing agent to the water phase to carry out the next round of polymerization . In the presence of limited oxygen, the method of the present invention does not require any modification of ligands, etc., and successfully realizes the efficient separation and recovery of ATRP and transition metal catalysts through simple stirring, diffusion and mass transfer. It is easy to operate, strong in designability, and relatively low in cost. Low, time-saving and labor-saving, it provides a new method for the simple, economical, efficient and environmentally friendly removal of ATRP catalysts.

Description

Technical field [0001] The present invention is a catalytic aggregate technology field. It specifically involves one atomic transfer aggregation method that can be efficiently recovered and recycled in a liquid / liquid system. Background technique [0002] Atom transfer free radical polymerization (ATRP) is a powerful "active" / controllable free radical polymerization method, which can precisely designs the macro structure and micro -structure of the polymer.Since the proposal in the 1990s, it has attracted great attention in the academic and industry (see K. Matyjaszewski, J. XIA, Chem. Rev., 2001, 101: 2921-2990 and M. Kamigaito, T. Ando, M. Sawamoto, Chem. Rev., 2001, 101: 3689-3746).Although ATRP can synthesize the polymer with a controllable molecular weight and a narrow molecular weight distribution, it must use a large amount of transition metal salt as a catalyst to regulate the growth process of polymerization.In this way, there are inevitable catalyst residues in the poly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F112/08C08F2/12C08F2/18C08F4/10
Inventor 程振平丁明强彭荩影姜孝武张丽芬朱秀林
Owner SUZHOU UNIV
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