Free radicalized ethylene-maleic anhydride copolymer and synthesis method thereof

A technology of maleic anhydride and synthesis method, which is applied in the field of free radical ethylene maleic anhydride copolymer and its synthesis, can solve the problems such as complicated reaction process, and achieve the effect of simple reaction, high molecular weight and mild conditions

Active Publication Date: 2018-06-22
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction process is cumbersome and requires multiple steps to obtain

Method used

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  • Free radicalized ethylene-maleic anhydride copolymer and synthesis method thereof
  • Free radicalized ethylene-maleic anhydride copolymer and synthesis method thereof
  • Free radicalized ethylene-maleic anhydride copolymer and synthesis method thereof

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[0030] The invention provides a kind of synthetic method of radicalized ethylene maleic anhydride copolymer, comprises the following steps:

[0031] Under the catalysis of the catalytic system, the ethylene-maleic anhydride copolymer and 4-hydroxyl-2,2,6,6-tetramethylpiperidine nitroxide radicals undergo an esterification reaction in a polar organic solvent to obtain Free radicalized ethylene maleic anhydride copolymer.

[0032] The present invention preferably carries out esterification reaction after mixing ethylene-maleic anhydride copolymer, 4-hydroxy-2,2,6,6-tetramethylpiperidine nitroxide free radical, catalytic system and polar organic solvent to obtain free Hydroxylated ethylene maleic anhydride copolymer. The present invention has no special limitation on the mixing mode of ethylene-maleic anhydride copolymer, 4-hydroxyl-2,2,6,6-tetramethylpiperidine nitroxide radical, catalytic system and polar organic solvent. A mixing method well known to those skilled in the art...

Embodiment 1

[0054] Solvent volume ratio:

[0055] Acetone: 70mL;

[0056] Ultra-dry dichloromethane: 10mL;

[0057] The proportion of reaction raw materials:

[0058] Commercial ethylene maleic anhydride copolymer (Mw=10,0000-45,0000) (PEM) 6mmol;

[0059] 4-Hydroxy-2,2,6,6-tetramethylpiperidine nitroxide radical (TEMPO-OH) 12mmol;

[0060] Catalyst 4-dimethylaminopyridine (DMAP): 3.6 mmol;

[0061] Acylating reagent 2-chloro-1-methylpyridinium iodide (CMPI): 6mmol;

[0062] Organic base triethylamine: 12mmol;

[0063] According to the proportioning ratio of substances, 6mmol ethylene maleic anhydride copolymer and 12mmol 4-hydroxyl-2,2,6,6-tetramethylpiperidine nitroxide radicals were completely dissolved in 40mL acetone; 3.6mmol DMAP was dissolved Add 30mL of acetone, and drop in the solution obtained above; add 18mmol of triethylamine, 6mmol of CMPI and 10mL of dichloromethane in sequence, and stir the reaction at room temperature in a nitrogen atmosphere; after reacting for 1 da...

Embodiment 2

[0065] Solvent volume ratio:

[0066] Acetone: 60mL;

[0067] Ultra-dry dichloromethane: 20mL;

[0068] The proportion of reaction raw materials

[0069] Commercial ethylene maleic anhydride copolymer (Mw=10,0000-45,0000) (PEM) 6mmol;

[0070] 4-Hydroxy-2,2,6,6-tetramethylpiperidine nitroxide radical (TEMPO-OH) 12mmol;

[0071] Catalyst 4-dimethylaminopyridine (DMAP): 3.6 mmol;

[0072] Acylating reagent 2-chloro-1-methylpyridinium iodide (CMPI) 6mmol;

[0073] Organic base triethylamine 12mmol;

[0074] According to the proportioning ratio of substances, 6mmol ethylene maleic anhydride copolymer and 12mmol 4-hydroxy

[0075] -2,2,6,6-Tetramethylpiperidine nitroxide completely dissolved in 40mL of acetone; 3.6mmol of DMAP was dissolved in 20mL of acetone, and dropped into the aforementioned solution; 18mmol of triethylamine, 6mmol of CMPI and 20mL dichloromethane, and stirred at room temperature in a nitrogen atmosphere; after 1 day of reaction, the mixed solvent in the...

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Abstract

The invention provides a synthesis method of a free radicalized ethylene-maleic anhydride copolymer, and belongs to the field of functional high molecular chemistry. An esterification reaction is performed on an ethylene-maleic anhydride copolymer and 4-hydroxy-2, 2, 6, 6-tetramethylpiperidine nitroxide free radicals to obtain the free radicalized ethylene-maleic anhydride copolymer. By the synthesis method, a previous method for preparing a free radicalized polymer by relying on complex and cumbersome monomer polymerization is broken through, only one step of simple esterification reaction isneeded, and the prepared free radicalized ethylene-maleic anhydride copolymer has high molecular weight and relatively high free radical content of per unit mass of repeating units, and the free radical number of each monomer molecule can be as high as 0.97; the electrolyte resistance is good, and the solubility in an electrolyte solution is only 0.59mg / mL; meanwhile, the synthesis method has theadvantages of simple reaction, mild condition, and high reaction degree which can reach 54%.

Description

technical field [0001] The invention relates to the field of functional polymer chemistry, in particular to a free radicalized ethylene maleic anhydride copolymer and a synthesis method thereof. Background technique [0002] As a new type of energy storage material, radicalized polymers have excellent properties such as fast charge and discharge rate, good cycle stability, and long service life, and have broad application prospects in the field of new energy. [0003] There are mainly two kinds of synthesis methods in the reported free radical polymers: one is to synthesize monomers with free radical side groups first, and then polymerize; the other is to synthesize monomers with piperidine structures, polymerize, And then further oxidation to obtain the corresponding free radical polymer. Xiaohuan Zhang et al. used the second method to prepare 4-propadienyl ether-2,2,6,6-tetramethylpiperidine monomer through a two-step reaction, then polymerized at 100°C, and then further ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/02C08F222/06C08F8/14
CPCC08F8/14C08F210/02C08F222/06
Inventor 章自寿陈耀光麦堪成
Owner SUN YAT SEN UNIV
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