Preparation method of polyimide and application of water-based lithium ion battery thereof

Abstract

The application discloses a preparation method of polyimide. The method comprises: carrying out a reaction on a solution containing a compound represented by a formula I and a compound represented bya formula II for 3-6 h at a temperature of 120-180 DEG C in an inactive atmosphere, performing separating, washing, and drying to obtain polyimide represented by a formula III; the method is simpler and more economical, and has the advantages of short reaction time, no high-temperature sintering, high yield and the like. The invention also discloses application of the polyimide prepared by the method in a water-based ion battery.

Description

technical field

[0001] The application relates to a preparation method of polyimide, which belongs to the field of polymer preparation. Background technique

[0002] Aqueous lithium-ion batteries are water-based battery systems. Because of its advantages such as high safety, environmental friendliness, and low cost, it has gradually attracted the attention of the large-scale energy storage market. Although the energy density of aqueous batteries is lower than that of traditional organic lithium-ion batteries, it is close to existing aqueous secondary batteries (such as lead-acid, nickel-cadmium batteries), and has both. At the system level, the water-based electrolyte does not ignite or explode at all, and does not require complicated battery management systems and thermal management systems, which can further save costs. Currently commercially used energy storage batteries are mainly lead-acid batteries and lithium iron phosphate or ternary power batteries. Among them, l...

Examples

Embodiment 1

[0081] The preparation of embodiment 1 polyimide

[0082] Step A: Add 1,4,5,8-naphthalene tetracarboxylic anhydride (NTCDA) powder and ethylenediamine (EDA) solution in the N-dimethylformamide (DMF) solution at a molar ratio of 1:1, keeping Magnetic stirring. The reaction concentration is 50g / 500ml. The reaction vessel is a glass flask. The flask was protected with argon. The flask was transferred to a 50°C oil bath, and the temperature was gradually raised to 150°C. The reaction was maintained at this temperature for 4 hours.

[0083] Step B: collect and centrifuge the products obtained by using method A and method B, and remove the supernatant. For the centrifuged sediment below, it was diluted and washed with N-dimethylformamide, and a second centrifugation was performed. Wash and centrifuge with ethanol. The final material was dried in a vacuum oven at 80° C. for 4 hours to obtain a dry powder, which was designated as polyimide sample 1.

Embodiment 2

[0084] The preparation of embodiment 2 polyimide

[0085] Step A: Add 1,4,5,8-naphthalene tetracarboxylic anhydride (NTCDA) powder and ethylenediamine solution (EDA) into the N-methylpyrrolidone (NMP) solution at a molar ratio of 1:1, and keep magnetic stirring . The reaction concentration is 50g / 500ml. The reaction vessel is a glass flask. The flask was protected with argon. The flask was transferred to a 50°C oil bath, and the temperature was gradually raised to 150°C. The reaction was maintained at this temperature for 4 hours.

[0086] Step B: collect and centrifuge the products obtained by using method A and method B, and remove the supernatant. For the centrifuged sediment below, dilute and wash with N-methylpyrrolidone, and perform a second centrifugation. Wash and centrifuge with ethanol. The final material was dried in a vacuum oven at 80° C. for 4 hours to obtain a dry powder, which was designated as polyimide sample 2.

Embodiment 3

[0087] The preparation of embodiment 3 polyimide

[0088] Step A: Add 1,4,5,8-naphthalene tetracarboxylic anhydride (NTCDA) powder and ethylenediamine solution (EDA) into the N-methylpyrrolidone (NMP) solution at a molar ratio of 1:1, and keep magnetic stirring . The reaction concentration is 50g / 300ml. The reaction vessel is a glass flask. The flask was protected with argon. The flask was transferred to a 50°C oil bath, and the temperature was gradually raised to 150°C. The reaction was maintained at this temperature for 6 hours.

[0089] Step B: collect and centrifuge the products obtained by using method A and method B, and remove the supernatant. For the centrifuged sediment below, dilute and wash with N-methylpyrrolidone, and perform a second centrifugation. Wash and centrifuge with ethanol. The final material was dried in a vacuum oven at 80° C. for 4 hours to obtain a dry powder, which was sintered at 350° C. for 8 hours under the protection of argon, which was r...

technical field

[0001] The application relates to a preparation method of polyimide, which belongs to the field of polymer preparation. Background technique

[0002] Aqueous lithium-ion batteries are water-based battery systems. Because of its advantages such as high safety, environmental friendliness, and low cost, it has gradually attracted the attention of the large-scale energy storage market. Although the energy density of aqueous batteries is lower than that of traditional organic lithium-ion batteries, it is close to existing aqueous secondary batteries (such as lead-acid, nickel-cadmium batteries), and has both. At the system level, the water-based electrolyte does not ignite or explode at all, and does not require complicated battery management systems and thermal management systems, which can further save costs. Currently commercially used energy storage batteries are mainly lead-acid batteries and lithium iron phosphate or ternary power batteries. Among them, l...

Examples

Embodiment 1

[0081] The preparation of embodiment 1 polyimide

[0082] Step A: Add 1,4,5,8-naphthalene tetracarboxylic anhydride (NTCDA) powder and ethylenediamine (EDA) solution in the N-dimethylformamide (DMF) solution at a molar ratio of 1:1, keeping Magnetic stirring. The reaction concentration is 50g / 500ml. The reaction vessel is a glass flask. The flask was protected with argon. The flask was transferred to a 50°C oil bath, and the temperature was gradually raised to 150°C. The reaction was maintained at this temperature for 4 hours.

[0083] Step B: collect and centrifuge the products obtained by using method A and method B, and remove the supernatant. For the centrifuged sediment below, it was diluted and washed with N-dimethylformamide, and a second centrifugation was performed. Wash and centrifuge with ethanol. The final material was dried in a vacuum oven at 80° C. for 4 hours to obtain a dry powder, which was designated as polyimide sample 1.

Embodiment 2

[0084] The preparation of embodiment 2 polyimide

[0085] Step A: Add 1,4,5,8-naphthalene tetracarboxylic anhydride (NTCDA) powder and ethylenediamine solution (EDA) into the N-methylpyrrolidone (NMP) solution at a molar ratio of 1:1, and keep magnetic stirring . The reaction concentration is 50g / 500ml. The reaction vessel is a glass flask. The flask was protected with argon. The flask was transferred to a 50°C oil bath, and the temperature was gradually raised to 150°C. The reaction was maintained at this temperature for 4 hours.

[0086] Step B: collect and centrifuge the products obtained by using method A and method B, and remove the supernatant. For the centrifuged sediment below, dilute and wash with N-methylpyrrolidone, and perform a second centrifugation. Wash and centrifuge with ethanol. The final material was dried in a vacuum oven at 80° C. for 4 hours to obtain a dry powder, which was designated as polyimide sample 2.

Embodiment 3

[0087] The preparation of embodiment 3 polyimide

[0088] Step A: Add 1,4,5,8-naphthalene tetracarboxylic anhydride (NTCDA) powder and ethylenediamine solution (EDA) into the N-methylpyrrolidone (NMP) solution at a molar ratio of 1:1, and keep magnetic stirring . The reaction concentration is 50g / 300ml. The reaction vessel is a glass flask. The flask was protected with argon. The flask was transferred to a 50°C oil bath, and the temperature was gradually raised to 150°C. The reaction was maintained at this temperature for 6 hours.

[0089] Step B: collect and centrifuge the products obtained by using method A and method B, and remove the supernatant. For the centrifuged sediment below, dilute and wash with N-methylpyrrolidone, and perform a second centrifugation. Wash and centrifuge with ethanol. The final material was dried in a vacuum oven at 80° C. for 4 hours to obtain a dry powder, which was sintered at 350° C. for 8 hours under the protection of argon, which was r...

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