Safe flame-retardant polyimide diaphragm and preparation method thereof

A polyimide and diaphragm technology, applied in the field of safe flame-retardant polyimide diaphragm and its preparation, can solve the problems of flammability, lithium-ion battery thermal runaway, smoke and fire, and achieve the effect of improving cycle performance

Active Publication Date: 2022-04-05
JIANGSU HORIZON NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under abnormal conditions such as overcharge, high-temperature storage, mechanical fracture, and penetration, an internal short circuit will occur between the positive and negative electrodes, resulting in thermal runaway inside the lithium-ion battery, resulting in explosion, smoke, and fire
Commercial separators represented by polyethylene (PE) and / or polypropylene (PP) have disadvantages such as poor thermal stability and flammability, and are technically difficult to meet the rapid development of lithium-ion batteries.

Method used

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  • Safe flame-retardant polyimide diaphragm and preparation method thereof
  • Safe flame-retardant polyimide diaphragm and preparation method thereof
  • Safe flame-retardant polyimide diaphragm and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Preparation of phosphorus-containing pentaerythritol flame retardant:

[0047] (1.1) Add 300mL of solvent dioxane and 65g of pentaerythritol to a 500mL three-necked flask successively, under the protection of nitrogen atmosphere, heat up and stir to 83°C, add 43mL of phosphorus oxychloride dropwise, heat up to 100°C, condense and reflux for 16h ; Filter, wash once with dioxane, wash twice with n-hexane, and dry to obtain intermediate product 1;

[0048] (1.2) Add 50mL o-dichlorobenzene, 25g pentaerythritol, 35mL phosphorus trichloride, and 0.15mL catalyst triethylamine successively in a 250mL three-necked flask. 100°C, kept at a constant temperature for 1 hour to obtain intermediate product 2;

[0049] Add 50g of intermediate product 1 directly, and then add 20g of sodium hydroxide to neutralize the HCl produced by the reaction to promote the positive direction of the reaction. Stop heating after 3 hours of reaction; filter, wash with dimethyl sulfoxide for 3 times...

Embodiment 2

[0057] (1) Preparation of phosphorus-containing pentaerythritol flame retardant:

[0058] (1.1) Add 300mL of solvent dioxane and 65g of pentaerythritol to a 500mL three-necked flask successively, under the protection of nitrogen atmosphere, heat up and stir to 80°C, add 57.5g of phosphorus oxychloride dropwise, heat up to 95°C, condense and reflux 15.5h; filter, wash once with dioxane, wash twice with n-hexane, and dry to obtain intermediate product 1;

[0059] (1.2) Add 50mL of o-dichlorobenzene, 25g of pentaerythritol, 57.5g of phosphorus trichloride, and 36.2g of catalyst triethylamine into a 250mL three-necked flask in sequence. Under the protection of nitrogen atmosphere, heat in an oil bath, and raise the temperature of the system within 3 hours to 95°C and kept at constant temperature for 1 hour to obtain intermediate product 2;

[0060] Directly add 50g of intermediate product 1, then add 20g of sodium hydroxide to neutralize the HCl produced by the reaction to promot...

Embodiment 3

[0068] (1) Preparation of phosphorus-containing pentaerythritol flame retardant:

[0069] (1.1) Add 300mL of solvent dioxane and 65g of pentaerythritol to a 500mL three-necked flask successively, under the protection of nitrogen atmosphere, heat up and stir to 85°C, add 70.8g of phosphorus oxychloride dropwise, heat up to 105°C, condense and reflux 16.5h; filter, wash once with dioxane, wash twice with n-hexane, and dry to obtain intermediate product 1;

[0070] (1.2) Add 50mL of o-dichlorobenzene, 25g of pentaerythritol, 57.7g of phosphorus trichloride, and 36.6g of catalyst triethylamine into a 250mL three-necked flask in sequence. Under the protection of nitrogen atmosphere, heat the oil bath, and raise the temperature of the system within 3 hours to 105°C, and kept at constant temperature for 1 hour to obtain intermediate product 2;

[0071] Directly add 50g of intermediate product 1, then add 20g of sodium hydroxide to neutralize the HCl produced by the reaction, promote...

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Abstract

The invention discloses a safe flame-retardant polyimide diaphragm and a preparation method thereof, and the preparation method comprises the following preparation processes: (1) heating pentaerythritol and phosphorus oxychloride in dioxane for reaction to obtain an intermediate product 1; the method comprises the following steps: heating pentaerythritol and phosphorus trichloride to react in a system of orthodichlorobenzene and a catalyst triethylamine to obtain an intermediate product 2; directly adding an intermediate product 1 and sodium hydroxide into the system, and reacting to obtain the phosphorus-containing pentaerythritol flame retardant. (2) dissolving APP, melamine phosphate, a dispersing agent, a phosphorus-containing pentaerythritol flame retardant and a binder in ultrapure water to obtain flame-retardant slurry; and coating on the surface of a ceramic membrane, and drying to obtain the flame-retardant polyimide coated diaphragm. Phosphorus-containing pentaerythritol intumescent flame retardants are prepared from pentaerythritol and phosphorus trichloride and prepared into flame-retardant slurry, and the surface of a ceramic coating polyimide film is coated with the flame-retardant slurry, so that the safety performance of the prepared lithium ion battery is ensured, meanwhile, shuttling of lithium ions is not affected, and the cycle performance of the battery is facilitated.

Description

technical field [0001] The invention relates to the technical field of battery diaphragms, in particular to a safe flame-retardant polyimide diaphragm and a preparation method thereof. Background technique [0002] Due to its high specific energy density and stable cycle performance, lithium-ion batteries are considered to be one of the most promising power sources for electric vehicles. With the development of technology, the energy density of batteries continues to increase, but ensuring their safety performance is still a big problem, which seriously hinders the further practical application of batteries. Separators in batteries are considered a key component in ensuring battery safety. The separator maintains the separation between the positive and negative electrodes by acting as a physical barrier between the positive and negative electrodes while providing a channel for Li-ion shuttling. Under abnormal conditions such as overcharge, high-temperature storage, mechani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M50/403H01M50/451H01M50/40
CPCY02E60/10
Inventor 张学虎张立斌贡晶晶陈朝晖
Owner JIANGSU HORIZON NEW ENERGY TECH CO LTD
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