Quaternary ammonium salt-doped nitroxide free radical polymer and preparation method thereof

A technology of nitroxide free radicals and quaternary ammonium salts, which is applied in the field of electrode materials, can solve the problems of low redox capacity, low water solubility, and unstable doping state, etc., and achieve the improvement of charge and discharge speed and cycle performance, fast movement, The effect of increasing the total energy density

Inactive Publication Date: 2018-10-16
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The specific capacity of the positive electrode of the free radical polymer system reported so far has not greatly exceeded that of the existing inorganic metal oxides. The internal relationship between the structure of the free radical polymer and the electrochemical performance still needs to be studied. The redox capacity of the existing free radical polymer as an electrode material Low, low water solubility, unstable doping state, resulting in the decline of self-discharge and rechargeable performance of free radical polymer batteries

Method used

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  • Quaternary ammonium salt-doped nitroxide free radical polymer and preparation method thereof
  • Quaternary ammonium salt-doped nitroxide free radical polymer and preparation method thereof
  • Quaternary ammonium salt-doped nitroxide free radical polymer and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] (1) In the Schlenk reaction tube, mix 4-methacrylic acid-2,2,6,6-tetramethylpiperidinol ester (22.2mmol), methacryloxyethyltrimethylammonium chloride 2 (22.2mmol, 80% aqueous solution), and soluble in dilute hydrochloric acid (0.75mol / L -1 ) In 2-mercaptoethanol (3.5mmol), and then add 4,4'-azobis(4-cyanovaleric acid) (ABCVA) (2.2mmol). The reaction system was kept in an oxygen-free state through three freeze-thaw cycles to cause free radical copolymerization to occur, and the reaction mixture was stirred at 75°C for 24 hours.

[0037] (2) Cool the solution to room temperature, and add hydrogen peroxide (33.3 mmol, 30% aqueous solution), sodium tungstate (0.29 mmol), EDTA (0.1 mmol) and sodium hydroxide aqueous solution (11 ml, 10% by weight). After stirring the solution for 24 hours, the remaining hydrogen peroxide (33.3 mmol) was added. The total reaction time was 48 hours. The solution was dialyzed with water (MWCO=1,000 gmol-1), filtered, and then the product was free...

Embodiment 2

[0039] (1) Combine 4-acrylamido-2,2,6,6-tetramethylpiperidine and methacryloxyethyltrimethylammonium chloride in a molar ratio of 1:1, and 2-mercaptoethanol Dissolve it in dilute hydrochloric acid, add it to the Schlenk reaction tube, and add 4,4'-azobis(4-cyanovaleric acid) (ABCVA). The reaction system was kept in an oxygen-free state through three freeze-thaw cycles to cause free radical copolymerization to occur, and the reaction mixture was stirred at 75°C for 24 hours.

[0040] (2) Cool the solution to room temperature, and add hydrogen peroxide (30% aqueous solution), sodium tungstate, EDTA and sodium hydroxide aqueous solution (Wt=10%). After stirring the solution for 24 hours, the remaining hydrogen peroxide was added. The total reaction time was 48 hours. The solution was dialyzed with water (MWCO=1,000 g mol-1), filtered, and then the product was freeze-dried. The operation was repeated three times to obtain an orange powder.

Embodiment 3

[0042] (1) Combine 4-methacrylic acid-2,2,6,6-tetramethylpiperidinol ester and 4-vinylbenzyltrimethylammonium chloride in a molar ratio of 1:1, and 2-mercapto Ethanol is dissolved in dilute hydrochloric acid and added to the Schlenk reaction tube together, and then 4,4'-azobis(4-cyanovaleric acid) (ABCVA) is added. The reaction system was kept in an oxygen-free state through three freeze-thaw cycles to cause free radical copolymerization to occur, and the reaction mixture was stirred at 75°C for 24 hours.

[0043] (2) Cool the solution to room temperature, and add hydrogen peroxide (30% aqueous solution), sodium tungstate, EDTA and sodium hydroxide aqueous solution (Wt=10%). After stirring the solution for 24 hours, the remaining hydrogen peroxide was added. The total reaction time was 48 hours. The solution was dialyzed with water (MWCO=1,000 g·mol-1), filtered, and then the product was freeze-dried. The operation was repeated three times to obtain an orange powder.

[0044] In ...

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Abstract

The invention relates to a quaternary ammonium salt-doped nitroxide free radical polymer and a preparation method thereof. The quaternary ammonium salt-doped nitroxide free radical polymer is characterized in that an irregular copolymer is synthesized by a free radical polymerizing method, and the ratio of free radial polymer part to doping part is regulated; the method of introducing N<+> groupsinto the quaternary ammonium salt is a common method for controlling the charge transfer property; meanwhile, the water solubility of the free radical polymer can be increased, and the electrochemicalproperty of the free radical polymer used as the electrical device is improved. By doping the N<+> into the nitroxide free radical polymer, the quaternary ammonium salt-doped nitroxide free radical polymer has the advantages that the charge and discharge speed and stability of the free radical polymer are improved; the service life of the free radical polymer is prolonged, and the water solubility of the free radical polymer is improved; the novel free radical polymer with high energy density is developed.

Description

Technical field [0001] The invention relates to the technical field of electrode materials, in particular to a quaternary ammonium salt doped nitroxide radical polymer and a preparation method thereof. Background technique [0002] In order to make solar, wind, and hydroelectric power generation and other renewable energy can be effectively used in the future, it is necessary to explore flexible and scalable energy storage solutions. At present, the secondary battery mainly uses inorganic oxide as the electrode material of the lithium ion battery. Considering safety and cost, energy density and capacity, especially with regard to the long-term use of metal resources, this puts a certain limit on lithium ion, and faces resources and Environmental issues call for new alternatives. Free radical polymer is a kind of organic polymer functional material containing stable free radicals. The stable free radicals in its structure can undergo rapid and reversible single-electron redox rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/34C08F8/06C08F220/60C08F226/02
CPCC08F8/06C08F220/34C08F220/60C08F226/02
Inventor 朱军峰拓欢覃智朱婷李俊国张光华
Owner SHAANXI UNIV OF SCI & TECH
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