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Polyvinyl pyridine preparing method

A technology of polyvinylpyridine and vinylpyridine, applied in the field of high-yield controllable synthesis, to achieve the effects of increasing polymerization rate and its controllability, controlling stereoregularity, and convenient post-processing

Inactive Publication Date: 2014-09-17
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, there is no public literature report on the high yield synthesis of vinylpyridine polymers at room temperature at home and abroad.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Under the condition of no ligand, ECPA is the initiator, and poly-4-vinylpyridine (P4VP) is synthesized in isopropanol solvent

[0040] Proportioned [4VP] 0 : [ECPA] 0 : [Cu(0)] 0 =256:1:1, sequentially add Cu(0), 4VP (1.0mL), isopropanol (1.0mL) and ECPA to a 5mL ampoule, add a stirring bar, and go through 6 times of standard freezing-pumping- After thawing and aerating cycles, seal the tubes in an oxygen-free atmosphere. The sealed ampoule was placed 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 isopropanol, pour it into 250 mL of n-hexane, leave it overnight, filter it with suction, and dry it to obtain poly-4-vinylpyridine.

Embodiment 2

[0041] Embodiment two: under the condition of no ligand, ECPA is initiator, synthesizes poly-4-vinylpyridine (P4VP) in HFIP solvent

[0042] Proportioned [4VP] 0 : [ECPA] 0 : [Cu(0)] 0 =256:1:1, sequentially add Cu(0), 4VP (1.0mL), HFIP (0.5~1.5mL) and ECPA to a 5mL ampoule, add a stirring bar, and go through 6 times of standard freezing-pumping- After thawing and aerating cycles, seal the tubes in an oxygen-free atmosphere. The sealed ampoule was placed 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 isopropanol, pour it into 250 mL of n-hexane, leave it overnight, filter it with suction, and dry it to get the "active" poly-4-vinyl pyridine.

[0043] The first line of data in Table 1 is the result of polymerization of 4-vinylpyridine monomer initiated by ECPA (4VP / isopropanol (v / v)=1 / 1).

[0044] figure 1 Under the condition of...

Embodiment 3

[0049] Embodiment three: with Me 6 -TREN as ligand, ECPA as initiator, poly-4-vinylpyridine (P4VP) was synthesized in isopropanol solvent

[0050] Proportioned [4VP] 0 : [ECPA] 0 : [Cu(0)] 0 : [Me 6 -TREN] 0 =256:1:1:1, add Cu(0), 4VP(1.0mL), Me 6 -TREN, isopropanol (1.0mL) and ECPA were placed in a 5mL ampoule, and a stirrer was added. After 6 standard freeze-pump-thaw inflation cycles, the tube was sealed under an oxygen-free atmosphere. The sealed ampoule was placed 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 isopropanol, pour it into 250 mL of n-hexane, leave it overnight, filter it with suction, and dry it to get the "active" poly-4-vinyl pyridine.

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Abstract

The invention relates to a high-yield controllable polyvinyl pyridine synthetic method at room temperature, which includes the steps: firstly, configuration of a reaction system, wherein the reaction system comprises polyvinyl pyridine monomer, initiator, a catalyzing system and solvent, the mole ratio of the polyvinyl pyridine monomer, the initiator and the catalyzing system is 100-1000:1:1, and the mole ratio of the monomer to the solvent is 1:0.5-3; and secondly, preparation of polyvinyl pyridine by 'activity' / controllable free radical polymerization reaction at 20-30 DEG C. The polyvinyl pyridine polymer is successfully synthetized at the room temperature for the first time by the method, the yield can reach more than 90%, and the precision structure of copolymerized compound is successfully regulated. Further, the polymerization system can be operated without ligand, less zero-valent copper powder is used as catalyst, post-treatment is convenient, and industrial production is facilitated.

Description

technical field [0001] The invention relates to a high-yield controllable synthesis method of polyvinylpyridine at room temperature. Background technique [0002] Free radical polymerization was developed in the 1950s and has become an important technology for industrial production of polymer products. However, although ordinary free radical polymerization is simple to operate, it has important defects such as poor molecular design ability and difficult control of polymer molecular weight and distribution, which makes it powerless to synthesize functional polymers with high performance and complex structure. So far, the relatively mature polymerization systems are: Initiator-transfer agent-terminator (Iniferter), stable free radical polymerization (Stable Free Radical Polymerization, SFRP), atom transfer radical polymerization (Atom Transfer Radical Polymerization) , ATRP) and reversible addition-fragmentation chain transfer polymerization (Reversible Addition Fragmentation...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F126/06C08F2/06C08F4/50
Inventor 朱秀林王文香张正彪程振平周年琛
Owner SUZHOU UNIV