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Synthesis of organic free radical polyalcohol PTMA anode material of lithium secondary battery and uses of the same

A lithium secondary battery and positive electrode material technology, which is applied in the synthesis process of free radical polymer PTMA, can solve the problems of poor fast charge and discharge performance, capacity attenuation, and structural instability, and achieve biodegradability and capacity attenuation The effect of slowing down and eliminating potential safety hazards

Inactive Publication Date: 2008-02-27
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The free radical polymer repeatedly undergoes oxidation-reduction reactions during the charge-discharge cycle, that is, electron transfer reactions occur with the current collector, while its molecular chain structure does not change, and no single anion and cation are generated during the redox process. Free radicals, it is neither like organic sulfides that will break the S-S bond during the charge-discharge cycle and become a small molecular substance that dissolves in the electrolyte or the structure is destroyed, resulting in capacity fading, nor like inorganic layered transition metals Due to the intercalation and intercalation of lithium ions during the charge and discharge of oxides, their structures are unstable, resulting in capacity decay and poor rapid charge and discharge performance during charge and discharge cycles.

Method used

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  • Synthesis of organic free radical polyalcohol PTMA anode material of lithium secondary battery and uses of the same
  • Synthesis of organic free radical polyalcohol PTMA anode material of lithium secondary battery and uses of the same
  • Synthesis of organic free radical polyalcohol PTMA anode material of lithium secondary battery and uses of the same

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Experimental program
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Effect test

Embodiment 1

[0043] (1) Chemical pretreatment process of raw materials, 2,2,6,6-tetramethyl-4-hydroxypiperidine (HTMP for short), recrystallized from benzene-ethanol, m.p.128~129℃; methyl methacrylate Ester (referred to as MMA), methyl methacrylate is dried by molecular sieve and then distilled for use; metallic copper (99.9%); magnesium powder (active magnesium content 99.0%); azobisisobutyronitrile (referred to as AIBN) is purified by ethanol crystallization Use; solvent tetrahydrofuran and ether with CaCl 2 After drying, it was used by refluxing with sodium benzophenone.

[0044] (2) The preparation process of the catalyst magnesium methoxide, adding magnesium powder and methanol in a reaction kettle with a stirrer, and then adding a small amount of iodine as an initiator. After 2 to 3 minutes of reaction at room temperature, the color of iodine faded and began to emit Hydrogen, after the reaction for 1 to 2 hours, no more hydrogen is released, the reaction solution becomes a white pas...

Embodiment 2

[0054] The PTMA obtained in Example 1 was used as an organic positive electrode material for a lithium secondary battery

[0055] (a) Assembly of the battery

[0056] The battery uses the PTMA aluminum foil electrode as the positive electrode and the metal lithium sheet as the negative electrode. The electrolyte is 1mol·L -1 LiPF 6 / EC-DMC (1:1 by volume). The assembly of the cells was carried out in an argon-filled glove box.

[0057] (b) Working principle of PTMA / lithium secondary battery

[0058] The working principle of PTMA / lithium secondary battery refers to its charging and discharging principle, which is the same as that of lithium secondary battery. According to the ESR spectra of oxidized PTMA (4.2V) and reduced PTMA (3V), as well as the charge-discharge and CV curves of PTMA, PTMA is at E a，p = The oxidation peak at 3.644V is that the O-N group of PTMA is oxidized and loses an electron to form a positive ion salt with the O=N group and the electrolyte anion, ...

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Abstract

The invention discloses a synthesis of Li twice battery organic free radical polymer PTMA polar material and application, which comprises the following steps: choosing HTMP and MMA as forerunner; adopting optimum ester interchange synthesized method; preparing MTMP; choosing eldopaque or metal copper as inhibitor; choosing metallic sodium or magnesium methylate as accelerant; preparing MTMP; using MTMP as monomer; choosing AIBN trigger; polymerizing through free radical body in toluene solution; preparing polymer PMTMP; using Na2WO4-H2O2-EDTA as oxidant in the methanol solution; getting PTMA with side chain as nitrogen oxygen stabilizing free radical. This invention can eliminate safe hidden danger of temperature increment, which possesses good electrolytic solution mutual dissolving property.

Description

technical field [0001] The invention relates to a synthesis process of a free-radical polymer PTMA (poly4-methacrylic acid-2,2,6,6-tetramethylpiperidine-1-nitroxide radical) and its application. Background technique [0002] Since the discovery of nitroxide-stabilized free radicals in 1956, nitroxide-stabilized free radicals have been widely used in cancer chemistry, radiation chemistry, excited state chemistry and spin labeling due to their special stability. The study of nitroxide-stabilized free radicals has become a very active field in free radical chemistry and biochemistry and has developed rapidly. [0003] Among the nitroxide-stabilized radicals, the most studied and most promising is the 2,2,6,6-tetramethyl-4-hydroxypiperidine-1-oxyl radical (2,2,6,6-tetramethyl-4 -piperidine-1-oxyl, referred to as TEMPO) and its derivatives. The synthesis of its ester derivatives has been reported. K.Murayama et al. synthesized 4-methacryloxy-2,2,6,6-tetramethylpiperidinol ester...

Claims

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Application Information

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IPC IPC(8): C08F120/10H01M4/60H01M4/66
CPCY02E60/12Y02E60/10
Inventor 邓凌峰陈洪
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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