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Acetylacetone manganese-initiated RAFT (reversible addition fragmentation chain transfer) polymerization method

A technology of manganese acetylacetonate and RAFT, applied in the field of RAFT polymerization initiated by manganese acetylacetonate, can solve the problems of low conversion rate, high polymerization temperature, and no reports on initiation of polymerization.

Active Publication Date: 2013-09-11
ZHEJIANG KELI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, at higher temperatures (60°C or 80°C), Mn(acac) 3 Under the condition of cooperating with RX, the control of the molecular weight of PMMA polymer is realized, but the molecular weight distribution is wide, M w / M n Between 2.0 and 3.0 (K.Endo and A.Yachi, Polym.J., 2002, 34, 320); at 80°C, Mn(acac) 3 Combined with BzBr, the molecular weight of PSt polymer can also be controlled, but the conversion rate is lower than 60%, M w / M n Between 2.0 and 3.0 (K. Endo and A. Yachi, Polym. Bull. 2001, 46, 363)
The above acetylacetonate (Mt(acac) x ) The polymerization reaction initiated by ) has poor control over the molecular weight, and the polymerization temperature is high
So far, acetylacetonate (Mt(acac) x ) has not been reported as an initiator of RAFT polymerization, and the initiation of polymerization at low temperature (room temperature) has not been reported

Method used

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  • Acetylacetone manganese-initiated RAFT (reversible addition fragmentation chain transfer) polymerization method
  • Acetylacetone manganese-initiated RAFT (reversible addition fragmentation chain transfer) polymerization method
  • Acetylacetone manganese-initiated RAFT (reversible addition fragmentation chain transfer) polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1 Mn(acac) 3 Under the combined action of / MECTP, bulk synthesis of polyvinyl acetate (PVAc)

[0039] According to the ratio [VAc] 0 :[MECTP] 0 :[Mn(acac) 3 ] 0 =200:(0,0.5,1,2):(0,0.05,0.1,0.2,1,4), add Mn(acac) in turn 3 , VAc (1.0mL) and MECTP in a 5mL ampoule, add a stir bar, after 6 standard freeze-pump-thaw inflation cycles, seal the tube under an oxygen-free atmosphere. The sealed ampoule was placed in the RCT basic S25 magnetic stirrer (80°C) of IKA Company to react according to the predetermined time, and the rotation speed was 900rpm. After the reaction, take out the sealed tube, open the sealed tube, dissolve it with 2-5 mL of tetrahydrofuran, pour it into 250 mL of n-hexane, leave it overnight, filter it with suction, and dry it to obtain PVAc.

[0040] The data in the first to third rows in Table 1 is [MECTP] in Example 1 0 :[Mn(acac) 3 ] 0 =1:0.05 and 1:0.1 aggregation results; the data in the 8th to 11th rows are respectively without M...

Embodiment 2

[0046] Example 2 Under the joint action of AIBN / MECTP, bulk synthesis of PVAc

[0047] According to the ratio [VAc] 0 :[MECTP] 0 :[AIBN] 0 =200:1:(0.05,0.1,0.2,1,4), add AIBN, VAc (1.0mL) and MECTP in sequence to a 5mL ampoule, add a stirrer, and go through 6 times of standard freezing-pumping-thawing After the inflation cycle, seal the tube under an oxygen-free atmosphere. The sealed ampoule was placed in the RCT basic S25 magnetic stirrer (80°C) of IKA Company to react according to the predetermined time, and the rotation speed was 900rpm. After the reaction, take out the sealed tube, open the sealed tube, dissolve it with 2-5 mL of tetrahydrofuran, pour it into 250 mL of n-hexane, leave it overnight, filter it with suction, and dry it to obtain PVAc.

[0048] The data in the 4th to 7th rows in Table 1 is [MECTP] in Example 2 0 :[AIBN] 0 = 1:0.05 and 1:0.1 of the polymerization results of VAc.

[0049] Figure 5 Under the condition of different AIBN concentration in ...

Embodiment 3

[0055] Embodiment 3 Mn(acac) 3 Synthesis of polymethyl methacrylate (PMMA) under the combined action of / CPDN

[0056] Proportioned [MMA] 0 :[CPDN] 0 :[Mn(acac) 3 ] 0 =200:(0,0.5,1,2):(0,0.5,1,2), add Mn(acac) in turn 3 , CPDN, ​​MMA (1.0mL) and solvent (0.5mL dimethylsulfoxide (DMSO), N,N-dimethylformamide (DMF), toluene or bulk) in a 5mL ampoule, add a stirring bar, and After 6 standard freeze-pump-thaw aeration cycles, seal the tube in an oxygen-free atmosphere. Place the sealed ampoule in a magnetic water bath at a constant temperature (25°C) for a predetermined time to react. After the reaction, take out the sealed tube, open the sealed tube, dissolve it with 2-5 mL of tetrahydrofuran, pour it into 250 mL of methanol, leave it overnight, filter it with suction, and dry it to obtain PMMA.

[0057] The data in rows 1, 3, and 4 in Table 2 are DMSO as the solvent in Example 3 without adding Mn(acac) 3 Or the polymerization results of MMA in CPDN; the data in the 5th t...

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Abstract

The invention discloses an acetylacetone manganese-initiated RAFT (reversible addition fragmentation chain transfer) polymerization method which comprises the following steps of: preparing a bulk polymerization reaction system comprising a vinyl monomer, an initiator and a chain transfer agent or a solution polymerization reaction system comprising a vinyl monomer, an initiator, a chain transfer agent and a solvent; and performing a polymerization reaction at 25-100 DEG C to obtain a polymer, wherein the molar ratio of the vinyl monomer to the initiator to the chain transfer agent is 200:(0.2-4):(0.5-2), the molar ratio of the vinyl monomer to the solvent is (0.5-3):1, and the initiator is acetylacetone manganese. The method disclosed by the invention adopts acetylacetone manganese as an RAFT polymerization initiator for the first time, is suitable for a wide range of monomers, and is effective to methacrylates, vinyl acetates and styrene monomers; the temperature application range is wider, and the application universality is enhanced; and as an initiator, the acetylacetone manganese can realize a higher end group functional degree of the tail end of the polymer.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and relates to a method for reversible addition-fragmentation chain transfer polymerization (RAFT for short), in particular to a manganese acetylacetonate (Mn(acac) 3 ) initiated RAFT aggregation method. Background technique [0002] Over the past few decades, there has been an increasing interest in polymer engineering. In terms of the synthesis of new polymeric materials with well-defined molecular parameters, controlled radical polymerization is a suitable method due to its mild reaction conditions and certain water resistance. At present, nitroxide-mediated polymerization (NMP for short), atom transfer radical polymerization (ATRP for short) and RAFT polymerization are among the most popular polymerizable monomers with a wide range. Controlled radical polymerization method. Among them, RAFT polymerization is usually carried out under the action of traditional free radical initiat...

Claims

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Application Information

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IPC IPC(8): C08F118/08C08F120/14C08F112/08C08F2/38C08F4/80
Inventor 张正彪王文香朱秀林周媛周年琛朱健程振平
Owner ZHEJIANG KELI NEW MATERIAL TECH CO LTD
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