Rare earth phthalocyanine sandwich layered structured negative electrode material and preparation method thereof

A technology of negative electrode material and sandwich layer, applied in the field of rare earth phthalocyanine sandwich layer structure compound, can solve problems such as battery performance degradation

Active Publication Date: 2018-08-17
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above existing problems, the present invention provides a rare earth metal complexed sandwich phthalocyanine layered negative electrode material, which solves the problem of battery performance attenuation caused by the instability of the layered structure in the prior art. Stabilize the layered structure to improve the structural stability of the material during the charge and discharge process, coupled with the high conductivity of the phthalocyanine macrocyclic conjugated structure, it can take into account the three advantages of large capacity, high conductivity and stable performance

Method used

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  • Rare earth phthalocyanine sandwich layered structured negative electrode material and preparation method thereof
  • Rare earth phthalocyanine sandwich layered structured negative electrode material and preparation method thereof
  • Rare earth phthalocyanine sandwich layered structured negative electrode material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0121] Synthesis Example 1: Solid phase synthesis of 4-nitroyttrium phthalocyanine

[0122] (1) Weigh 4-nitrophthalic anhydride (0.1mol), anhydrous YCl 3 (0.0125mol), ammonium molybdate (0.002mol) and urea (4mol), grind them into fine particles with a mortar, and then mix them together, and continue grinding until the powder particles of each component are mixed uniformly to obtain a mixed raw material , and finally transferred to a 500ml beaker;

[0123] (2) Cover the beaker containing the mixed raw materials with a glass cover, place it in an oven and heat it slowly to 150°C, and keep it warm for 30 minutes. At this time, there will be bubbles inside the beaker;

[0124] (3) After no bubbles are generated in the beaker, the temperature of the system is raised to 190° C., and the reaction is carried out at a constant temperature for 5 hours. After cooling, a blue-black solid product is obtained in the beaker;

[0125] (4) Scrape the black solid from the beaker, crush it wit...

Embodiment 2

[0135] Synthesis Example 2: Liquid phase synthesis of 4-nitroyttrium phthalocyanine

[0136] (1) The 4-nitrophthalonitrile that takes 0.1mol joins in the there-necked flask that fills 200ml n-amyl alcohol, feeds N 2 And keep stirring, raise the temperature to 60°C, and keep it warm for 3h;

[0137] (2) Weigh 0.0125mol anhydrous YCl 3 Quickly add it into the three-necked bottle, then draw 1,8-diazabicycloundec-7-ene (DBU) catalyst with a disposable dropper, and drop 5 drops into the three-necked bottle, continue to pass through the N 2 Stir for 30min;

[0138] (3) Slowly raise the temperature to 140°C, and reflux at this temperature for 36 hours, the mixed solution gradually turns into a blue solution;

[0139] (4) After the reaction solution is cooled, it is poured into ethanol and stirred for 30 min, left to settle, filtered, and dried to obtain a blue-black solid phthalocyanine compound.

[0140] (5) The black phthalocyanine solid powder obtained above was recrystallized...

Embodiment 3

[0143] Synthesis Example 3: Solid Phase Synthesis of 4-Nitroeuropium Phthalocyanine

[0144] (1) Weigh 4-nitrophthalic anhydride (0.1mol), anhydrous EuCl 3 (0.0167mol), ammonium molybdate (0.003mol) and urea (6mol), grind them into fine particles with a mortar, and then mix them together, and continue grinding until the powder particles of each component are mixed uniformly to obtain a mixed raw material , and finally transferred to a 500ml beaker;

[0145] (2) Cover the beaker containing the mixed raw materials with a glass cover, place it in an oven and heat it slowly to 160°C, and keep it warm for 20 minutes. At this time, there will be bubbles inside the beaker;

[0146] (3) After no bubbles are generated in the beaker, the temperature of the system is raised to 200° C., and the reaction is carried out at a constant temperature for 8 hours. After cooling, a blue-black solid product is obtained in the beaker;

[0147] (4) The black solid was scraped out from the beaker, c...

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Abstract

The invention discloses a rare earth phthalocyanine sandwich layered structured compound and a preparation method thereof. According to the method, a "solid phase" or a "liquid phase" template synthesis method is adopted to synthesize the compound in one step, and then through a purification technology with a combination of specifically designed recrystallization, washing and thermal vacuum treatment, the high-purity rare earth phthalocyanine sandwich layered structured compound is obtained, wherein the layer spacing of the compound is 2-4angstroms, and effective reversible intercalation and deintercalation of lithium ions can be realized. The synthesis technology disclosed in the invention has high yield, less side products, high target compound purity, simple operation process and low cost and is suitable for industrial large-scale production; the capacity of the negative electrode material is obviously higher than the theoretical capacity (372 mAh / g) of the conventional graphite negative electrode material; in addition, the negative electrode material has very high initial coulombic efficiency and cycle performance; and therefore, the lithium ion battery assembled by taking therare earth phthalocyanine sandwich layered structured compound as the negative electrode material has excellent electrochemical performance and practical value.

Description

【Technical field】 [0001] The present invention relates to a rare earth phthalocyanine sandwich layered structure compound and a synthesis method of the compound; in addition, the present invention also relates to the application of the negative electrode material of the rare earth phthalocyanine sandwich layered structure compound lithium ion battery, and the A lithium ion battery using a rare earth phthalocyanine sandwich layer structure compound as a negative electrode material and a preparation method of the lithium ion battery. 【Background technique】 [0002] With the increasing demand for energy and the deepening awareness of the importance of sustainable social and economic development, the requirements for lithium-ion battery electrode materials are also getting higher and higher. In lithium-ion batteries, as a two-dimensional lithium ion intercalation / extraction layered structure material, it has the advantages of capacity, rate performance and conductivity that othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/60H01M4/137H01M10/0525
CPCH01M4/137H01M4/602H01M10/0525Y02E60/10
Inventor 陈军徐勇曹米红
Owner JIANGXI UNIV OF SCI & TECH
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