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A preparation method of interpenetrating network polymer electrolyte containing n and p atoms

A technology of interpenetrating network and polymer, applied in the field of interpenetrating network polymer electrolyte and its preparation

Active Publication Date: 2021-01-05
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are very few polymer electrolytes that can reach this level, so it is very important to prepare polymer electrolytes that meet the conductivity requirements of lithium-ion batteries.

Method used

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  • A preparation method of interpenetrating network polymer electrolyte containing n and p atoms
  • A preparation method of interpenetrating network polymer electrolyte containing n and p atoms

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0005] (1) Preparation of ethanolamine-epichlorohydrin dendrimers

[0006] In the three-necked reaction flask, add 0.050mol ethanolamine, 0.050mol lithium hydroxide and 20ml distilled water, stir and dissolve at 25°C, raise the temperature to 90°C, slowly add 0.200mol epichlorohydrin dropwise, after the addition, continue the heat preservation reaction for 6h, After cooling to room temperature, a yellow viscous liquid was obtained;

[0007] (2) preparation of two-maleic acid monopolyethylene glycol ester

[0008] Put 0.050mol maleic anhydride, 0.025mol polyethylene glycol-6000 and 1.000g p-toluenesulfonic acid in a 100ml three-necked reaction flask with a condenser and a water separator, heat to 105°C to melt, and stir for 5 hours , separate the water, pour it into a beaker while it is hot, and cool to room temperature to obtain a waxy solid;

[0009] (3) Preparation of interpenetrating network polymer

[0010] Add the samples prepared in the above (1) and (2) into 100ml of...

Embodiment 2

[0012] (1) Polymer gel strength

[0013] Take the sample of Example 1 (3), adjust the shear rate of the rheometer to 500S-1 at different temperatures, and measure the strength of the gel. See Table 1.

[0014] Table 1 The shear strength of polymer gel (shear rate: 500S -1 )

[0015] temperature, ℃ -20 -10 0 10 20 50 80 Shear strength, Pa 25.54 24.39 23.1 20.36 17.42 15.31 8.22

[0016] (2) Polymer water absorption

[0017] Accurately get the samples of Example 1 (3) and place them in 5% lithium chloride aqueous solution respectively, then seal it at a certain temperature and soak for a certain period of time, wipe off the surface moisture, and measure the water absorption rate of the polymer at different times. See Table 2.

[0018] Table 2 Water absorption of polymers

[0019]

[0020] (3) Polymer molding shrinkage

[0021] The sample in Example 1(3) was heated to 100°C, and a mold with a dial indicator (accuracy of 0.01mm) was used t...

Embodiment 3

[0030] Before the system is cooled, the polymer electrolyte membrane of Example 1 (3) of a certain size is sandwiched between two metal electrodes, and the measurement line is connected. The electrode area A and the thickness d of the polymer electrolyte membrane were measured. Set the sweep frequency range from 1Hz to 10 5 Hz, using a Solartron SI1287+SI1260 electrochemical comprehensive tester to measure the AC impedance spectrum of the sample at a temperature of -20°C to 25°C. From the intersection point of the tail line and the real axis in the AC impedance spectrum, read the resistance Rb of the gel sample, and calculate the conductivity of the polymer electrolyte according to the formula: σ=d / (Rb·A). see table 5

[0031] Table 5 Ionic conductivity of gel at different temperatures

[0032] temperature, ℃ -20 -10 0 10 25 Ionic conductivity, S / cm 5.50×10 -6

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Abstract

The invention relates to a preparation method of an interpenetrating network polymer electrolyte prepared by using lithium acrylate, maleic anhydride, lithium hypophosphite, lithium allylsulfonate, polyethylene glycol-6000, ethanolamine and epichlorohydrin as raw materials. The preparation method comprises the following steps: firstly initiating polymerization of ethanolamine and epichlorohydrin in an aqueous medium by the use of lithium hydroxide to prepare an aqueous solution of ethanolamine-epichlorohydrin dendrimer, and then preparing bis-maleic acid monopolyethylene glycol ester-6000 by using maleic anhydride and polyethylene glycol as raw materials; adding bis-maleic acid monopolyethylene glycol ester-6000, lithium acrylate, lithium hypophosphite and lithium allylsulfonate into the aqueous solution of ethanolamine-epichlorohydrin dendrimer, and initiating polymerization by the use of hydrogen peroxide and ammonium ferric sulfate to prepare the interpenetrating network polymer electrolyte containing phosphorus atoms and nitrogen atoms.

Description

technical field [0001] The invention belongs to the field of gel electrolytes, in particular to a lithium acrylate, maleic anhydride, lithium hypophosphite, lithium allyl sulfonate, polyethylene glycol-6000, ethanolamine and epichlorohydrin as raw materials The prepared interpenetrating network polymer electrolyte and its preparation method. Background technique [0002] The key to polymer electrolytes is to increase the ionic conductivity to 10% of the room temperature ionic conductivity required for lithium-ion batteries. -3 S / cm level. Its main development directions include single-ion polymer electrolytes, network polymer electrolytes suspended with polyether chains, and two-phase polymer electrolytes. However, there are very few polymer electrolytes that can reach this level at present, so it is very important to prepare polymer electrolytes that meet the conductivity requirements of lithium-ion batteries. The present invention integrates three development directions...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0565H01M10/0525C08F283/06C08F283/10C08F228/02C08F220/06
CPCC08F283/065C08F283/10H01M10/0525H01M10/0565C08F228/02Y02E60/10
Inventor 麻金海孔淑玲方龙
Owner QINGDAO UNIV