CN112038695A - Flame-retardant solid polymer electrolyte modified by phosphotriester solution and preparation method thereof - Google Patents
Flame-retardant solid polymer electrolyte modified by phosphotriester solution and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a flame-retardant solid polymer electrolyte modified by a phosphoric triester solution and a preparation method thereof. The introduced phosphoric acid triester solution generates a phosphoric acid group with flame retardant effect after being heated and decomposed, and has great contribution to improving the flame retardant property of the electrolyte. The flame-retardant solid polymer electrolyte modified by the phosphotriester solution prepared by the method has good ionic conductivity and electrochemical stability, and excellent flame-retardant property, and can greatly improve the safety of the battery when being applied to the all-solid-state lithium battery.
Description
Technical Field
The invention belongs to the field of lithium battery electrolytes, and relates to a flame-retardant solid polymer electrolyte modified by a phosphotriester solution and a preparation method thereof.
Background
With the vigorous development of renewable energy sources in various countries in the world, the lithium battery serving as the most efficient energy storage device has huge market potential. With the increasing demand of life and production, how to realize faster charging and higher energy density is a necessary trend of lithium battery development. Solid-state lithium batteries are considered as one of the directions for the development of lithium batteries in the future, and solid-state electrolytes have been widely researched and pursued as core members of solid-state batteries. Among them, the solid polymer electrolyte is considered as a breakthrough point of the solid electrolyte due to simple preparation process, good flexibility and good interface compatibility, and the most interesting polymer matrix is ethylene oxide (PEO), but the flammability of PEO is often ignored, especially when the PEO is applied to a lithium battery, the flammability of PEO is easily amplified under the condition of thermal runaway, and an irrecoverable safety accident is caused.
The phosphoric triester solution is a phosphorus flame retardant, when the phosphoric triester solution is applied to a solid polymer electrolyte, the flame retardant mechanism is that a flame retardant additive releases free radicals with flame retardant property when being heated, and the free radicals can capture hydrogen free radicals or hydroxyl free radicals in a gas phase, so that the chain reaction of the hydroxyl free radicals is prevented, the combustion cannot be carried out or is difficult to carry out, and the safety performance of the lithium battery is improved.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a phosphoric triester solution modified flame-retardant solid polymer electrolyte and a preparation method thereof.
Technical scheme
A flame-retardant solid polymer electrolyte modified by a phosphoric triester solution, which is characterized in that: the preparation method comprises the following steps of taking a phosphotriester solution as a modified liquid, polyethylene oxide (PEO) as a matrix, and lithium perchlorate or lithium bis (trifluoromethanesulfonyl) imide as a lithium salt, wherein: PEO: Li+The molar ratio of (A) to (B) is 10: 1-17: 1; the dosage of the phosphoric triester solution is 2-3 times of the total mass of the polymer matrix and the lithium salt.
The phosphoric triester solution is any one or a mixed solution of trimethyl phosphate TMP and triethyl phosphate TEP.
The PEO: Li+The molar ratio of (A) to (B) is 15: 1.
The molecular weight range of the polyethylene oxide (PEO) is 600000-1000000.
The molecular weight of the polyethylene oxide PEO is 1000000.
A preparation method of the flame-retardant solid polymer electrolyte modified by the phosphoric acid triester solution is characterized by comprising the following steps:
step 1: weighing PEO, LiTFSI or LiClO in proportion4Dissolving the phosphoric triester solution in acetonitrile, and magnetically stirring the solution until the solution is uniform; the acetonitrile accounts for 8-9 times of the total mass;
step 2: and (3) casting the solution in a polytetrafluoroethylene culture dish, volatilizing at room temperature to remove the solvent, and drying at 40-70 ℃ for 6-24 h to obtain the phosphotriester solution modified flame-retardant solid polymer electrolyte.
The stirring speed of the step 1 is 400-600 rpm.
The stirring speed in step 1 was 530 rpm.
The stirring time in the step 1 is 6-18 h.
The drying time of the step 2 is 12-18 hours, and the drying temperature is 60 ℃.
Advantageous effects
The invention provides a phosphoric triester solution modified flame-retardant solid polymer electrolyte and a preparation method thereof. The introduced phosphoric acid triester solution generates a phosphoric acid group with flame retardant effect after being heated and decomposed, and has great contribution to improving the flame retardant property of the electrolyte. The flame-retardant solid polymer electrolyte modified by the phosphotriester solution prepared by the method has good ionic conductivity and electrochemical stability, and excellent flame-retardant property, and can greatly improve the safety of the battery when being applied to the all-solid-state lithium battery.
FIG. 1 is a graph showing the results of testing combustion of a sample of the product of example 1 of the present invention. The results of fig. 1 show that the prepared solid polymer electrolyte membrane did not ignite after the addition of the phosphotriester-based solution, and showed excellent flame retardancy.
FIG. 2 is a scanning electron micrograph of a sample of the product of example 2 of the present invention. The components of the obtained electrolyte membrane are uniformly dispersed and do not agglomerate as can be seen from a scanning electron microscope image, which shows that the added phosphotriester solution does not change other properties of the electrolyte membrane.
FIG. 3 is a graph of the results of a Linear Sweep Voltammetry (LSV) test on a sample of the product of example 3 of the present invention. LSV tests show that the electrochemical stability window of the phosphoric acid triester solution modified PEO-based flame-retardant solid polymer electrolyte reaches 4.86V, and the electrolyte can be matched with almost all electrode materials in the current stage.
FIG. 4 is a plot of electrochemical impedance at 55 ℃ of a sample of the product of example 4 of the present invention. From the graph, it can be read that the lithium ion conduction resistance value is about 43ohm, which is close to the value of the commercial liquid electrolyte.
FIG. 5 is a charge and discharge test curve at 55 ℃ for a sample of the product of example 5 of the present invention. With lithium iron phosphate (LiFePO)4) And lithium metal is used as an electrode material, and a charging and discharging test is carried out on the phosphate triester solution modified PEO-based flame-retardant solid polymer electrolyte assembled battery. The first turn coulombic efficiency is close to 100%, which is better than the test result of the traditional commercial liquid electrolyte.
Compared with the prior art, the flame retardance is greatly improved on the premise of not greatly improving the cost by introducing the phosphotriester solution as the modified solution, the electrochemical stability and the ionic conductivity are improved, and powerful guarantee is provided for preparing the core component of the all-solid-state lithium battery with high safety.
Drawings
FIG. 1 is a graph of the results of combustion testing of product samples of example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a sample of the product of example 2 of the present invention.
FIG. 3 is a graph of the results of linear sweep voltammetry tests on a sample of the product of example 3 of the present invention.
FIG. 4 is an electrochemical impedance spectrum of a sample of the product of example 4 of the present invention.
FIG. 5 is a charge and discharge test curve at 55 ℃ for a sample of the product of example 5 of the present invention.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the following is a detailed description of a phosphoric acid triester solution modified flame retardant solid polymer electrolyte and a method for preparing the same according to an embodiment of the present invention.
Example 1:
step 1: mixing LiTFSI, PEO (M)w＝106g mol-1) And placing the trimethyl phosphate solution in a vacuum oven at 50 ℃ for drying for 24 hours, and placing the dried solution in a glove box for later use.
Step 2: weighing the PEO, the LiTFSI and the trimethyl phosphate solution obtained by drying in the step 1 according to the proportion, wherein the mass of the trimethyl phosphate solution is 2 times of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing off the film, placing the film in a polytetrafluoroethylene culture dish, drying the film in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based flame-retardant solid polymer electrolyte taking trimethyl phosphate solution as a modified solution.
Example 2:
step 1: mixing LiTFSI, PEO (M)w＝106g mol-1) And putting the triethyl phosphate solution into a vacuum oven at 50 ℃ for drying for 24 hours, and putting the solution into a glove box for later use.
Step 2: weighing the PEO, the LiTFSI and the triethyl phosphate solution obtained by drying in the step 1 according to the proportion, wherein the mass of the triethyl phosphate solution is 2 times of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine in a beaker, and adding acetonitrile (the weight of the weighed medicine is the weighed medicine)9 times of the total mass of the product), and strongly stirring at room temperature for 12 h.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing the membrane, placing the membrane in a polytetrafluoroethylene culture dish, drying the membrane in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based flame-retardant solid polymer electrolyte taking the triethyl phosphate solution as the modified solution.
Example 3:
step 1: mixing LiTFSI, PEO (M)w＝106g mol-1) Placing the trimethyl phosphate and the triethyl phosphate solution in a vacuum oven at 50 ℃ for drying for 24 hours, and placing the dried product in a glove box for later use.
Step 2: weighing a mixed solution of PEO, LiTFSI, trimethyl phosphate, triethyl phosphate and the like obtained by drying in the step 1 in proportion, wherein the mass of the mixed solution is 2 times of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing the film, placing the film in a polytetrafluoroethylene culture dish, drying the film in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based flame-retardant solid polymer electrolyte taking the mixed solution of trimethyl phosphate and triethyl phosphate as a modified solution.
Example 4:
step 1: LiClO is added4、PEO(Mw＝106g mol-1) And placing the trimethyl phosphate solution in a vacuum oven at 50 ℃ for drying for 24 hours, and placing the dried solution in a glove box for later use.
Step 2: weighing the PEO and the LiClO obtained by drying in the step 1 according to the proportion4And a trimethyl phosphate solution having a mass 2 times the total mass of the polymer substrate and the lithium salt, EO: li+In a molar ratio of 15: 1, placing the weighed medicines in a deviceAcetonitrile (the mass is 9 times of the total mass of the weighed medicines) is added into the beaker, and the mixture is stirred vigorously at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing off the film, placing the film in a polytetrafluoroethylene culture dish, drying the film in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based flame-retardant solid polymer electrolyte taking trimethyl phosphate solution as a modified solvent.
Example 5:
step 1: mixing LiTFSI, PEO (M)w＝6×105g mol-1) And placing the trimethyl phosphate solution in a vacuum oven at 50 ℃ for drying for 24 hours, and placing the dried solution in a glove box for later use.
Step 2: weighing the PEO, the LiTFSI and the trimethyl phosphate solution obtained by drying in the step 1 according to the proportion, wherein the mass of the trimethyl phosphate solution is 2 times of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing off the film, placing the film in a polytetrafluoroethylene culture dish, drying the film in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based flame-retardant solid polymer electrolyte taking trimethyl phosphate solution as a modified solution.
Claims (10)
1. A flame-retardant solid polymer electrolyte modified by a phosphoric triester solution, which is characterized in that: the preparation method comprises the following steps of taking a phosphotriester solution as a modified liquid, polyethylene oxide (PEO) as a matrix, and lithium perchlorate or lithium bis (trifluoromethanesulfonyl) imide as a lithium salt, wherein: PEO: Li+The molar ratio of (A) to (B) is 10: 1-17: 1; the dosage of the phosphoric triester solution is 2-3 times of the total mass of the polymer matrix and the lithium salt.
2. The triester phosphate solution modified flame retardant solid polymer electrolyte of claim 1, wherein: the phosphoric triester solution is any one or a mixed solution of trimethyl phosphate TMP and triethyl phosphate TEP.
3. The triester phosphate solution modified flame retardant solid polymer electrolyte of claim 1, wherein: the PEO: Li+The molar ratio of (A) to (B) is 15: 1.
4. The triester phosphate solution modified flame retardant solid polymer electrolyte of claim 1, wherein: the molecular weight range of the polyethylene oxide (PEO) is 600000-1000000.
5. The triester phosphate solution modified flame retardant solid polymer electrolyte of claim 1, wherein: the molecular weight of the polyethylene oxide PEO is 1000000.
6. A method for preparing a phosphoric acid triester solution modified flame retardant solid polymer electrolyte as claimed in any one of claims 1 to 5, characterized by comprising the steps of:
step 1: weighing PEO, LiTFSI or LiClO in proportion4Dissolving the phosphoric triester solution in acetonitrile, and magnetically stirring the solution until the solution is uniform; the acetonitrile accounts for 8-9 times of the total mass;
step 2: and (3) casting the solution in a polytetrafluoroethylene culture dish, volatilizing at room temperature to remove the solvent, and drying at 40-70 ℃ for 6-24 h to obtain the phosphotriester solution modified flame-retardant solid polymer electrolyte.
7. The method of claim 6, wherein: the stirring speed of the step 1 is 400-600 rpm.
8. The method of claim 6, wherein: the stirring speed in step 1 was 530 rpm.
9. The method of claim 6, wherein: the stirring time in the step 1 is 6-18 h.
10. The method of claim 6, wherein: the drying time of the step 2 is 12-18 hours, and the drying temperature is 60 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112625283A (en) * | 2020-12-18 | 2021-04-09 | 江汉大学 | Flame-retardant polyethylene oxide solid electrolyte membrane |
| CN113036216A (en) * | 2021-03-10 | 2021-06-25 | 西北工业大学 | Composite flame retardant modified PEO-based solid polymer electrolyte and preparation method thereof |
| CN114976236A (en) * | 2022-07-08 | 2022-08-30 | 福州大学 | Flame-retardant gel electrolyte for lithium metal and preparation method and application thereof |
| CN115332624A (en) * | 2022-10-13 | 2022-11-11 | 西北工业大学 | Preparation method of thermal-stable, ultrathin, light and flame-retardant PEO-based solid electrolyte |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625283A (en) * | 2020-12-18 | 2021-04-09 | 江汉大学 | Flame-retardant polyethylene oxide solid electrolyte membrane |
| CN112625283B (en) * | 2020-12-18 | 2022-05-27 | 江汉大学 | Flame-retardant polyethylene oxide solid electrolyte membrane |
| CN113036216A (en) * | 2021-03-10 | 2021-06-25 | 西北工业大学 | Composite flame retardant modified PEO-based solid polymer electrolyte and preparation method thereof |
| CN114976236A (en) * | 2022-07-08 | 2022-08-30 | 福州大学 | Flame-retardant gel electrolyte for lithium metal and preparation method and application thereof |
| CN115332624A (en) * | 2022-10-13 | 2022-11-11 | 西北工业大学 | Preparation method of thermal-stable, ultrathin, light and flame-retardant PEO-based solid electrolyte |
| CN115332624B (en) * | 2022-10-13 | 2023-01-31 | 西北工业大学 | Preparation method of heat-stable, ultrathin, light and flame-retardant PEO-based solid electrolyte |
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