CN112111079B - Dopamine-modified polyimide battery diaphragm and preparation method and application thereof - Google Patents
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Abstract
The invention belongs to the field of battery diaphragms, and discloses a dopamine-modified polyimide battery diaphragm, and a preparation method and application thereof. S1, soaking a carrier in the dopamine solution, and vibrating at room temperature until the dopamine solution and the carrier are uniformly mixed to obtain a carrier loaded with dopamine; s2, adding the dopamine-loaded carrier and the additive into a precursor polyamide acid PAA solution, and stirring to obtain a mixed solution, wherein the additive is one or more of polyethylene oxide, polypropylene oxide, polyethylene glycol, dimethyl phthalate, polymethyl methacrylate or polyurethane; s3, coating the mixed liquid on polytetrafluoroethylene, and performing chemical imidization or thermal imidization treatment to obtain the polyimide porous film, wherein the thermal imidization is performed according to the program steps of 100 ℃/1h, 200 ℃/1h and 300 ℃/1h for curing. Through the synergistic interaction between the dopamine and the carrier and the additive, the liquid absorption capacity of the battery diaphragm is improved, and the related performances such as the porosity of the battery diaphragm are improved.
Description
Technical Field
The invention relates to the technical field of battery diaphragms, in particular to a preparation method and application of a dopamine modified polyimide battery diaphragm.
Background
Lithium ion secondary batteries are a reusable battery, and are also a clean energy source, and are attracting attention of more and more researchers. The lithium battery consists of a positive electrode, a negative electrode, electrolyte, a battery diaphragm and 5 main components of a battery shell. The lithium ion battery diaphragm is a functional film which is arranged between the positive electrode and the negative electrode of the battery, and mainly aims to prevent the contact short circuit of the positive electrode and the negative electrode, and meanwhile, ions and charge carriers can be transported in a closed channel of the lithium ion battery. The commercial diaphragm has the problems of low porosity, poor wettability, no high temperature resistance and the like, and influences the charge-discharge capacity and the cycle performance of the lithium battery. The polyimide has excellent comprehensive performance, can be used for a long time at the temperature of up to 300 ℃, and the dopamine is easy to self-polymerize to form Polydopamine (PDA), has high adhesion, can increase the tensile strength of a battery film to avoid short circuit, and has the characteristics of increasing the liquid absorption rate and the like.
Chinese patent (CN 103545474 a) discloses a polydopamine modified lithium ion battery separator and a preparation method, wherein the method discloses a polydopamine modified polyimide lithium ion battery separator, and the solution comprises a polydopamine coating and a high polymer porous membrane matrix, and the polyimide high temperature resistant and strong dopamine binding power is utilized, so that the high temperature resistant capability is improved, and the electrolyte adsorption/retention capability is improved, but the porosity of the battery separator cannot be improved.
Disclosure of Invention
The invention aims to solve the technical problem of improving the porosity of a battery diaphragm and providing a dopamine modified polyimide battery diaphragm.
The invention further aims to provide a preparation method of the dopamine-modified polyimide battery separator.
It is another object of the present invention to provide the use of the dopamine modified polyimide battery separator in a battery separator.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the dopamine-modified polyimide battery diaphragm comprises the following steps:
s1, soaking a carrier in the dopamine solution, and vibrating at room temperature until the carrier is uniformly mixed; obtaining a carrier loaded with dopamine;
s2, adding the dopamine-loaded carrier and the additive into the prepared precursor polyamide acid PAA solution, and fully stirring to obtain a mixed solution, wherein the additive is one or more of polyethylene oxide, polypropylene oxide, polyethylene glycol, dimethyl phthalate, polymethyl methacrylate or polyurethane;
s3, coating the mixed solution on polytetrafluoroethylene, and performing chemical imidization or thermal imidization treatment, wherein the thermal imidization is performed according to the program step-type heating solidification of 100 ℃/1h, 200 ℃/1h and 300 ℃/1 h.
The shaking is carried out by a water bath or an air bath shaking table, and the shaking time is 24-48 hours.
The invention carries dopamine on carrier, then mixes with precursor polyamic acid and additive to proceed thermal imidization treatment or chemical imidization treatment. The dopamine polyimide film is obtained by a chemical imine method in the step S3, the dopamine can increase the liquid absorption rate, has high adhesion effect, can enhance the combination of a carrier and the polyimide film, and can also be reheated to 300 ℃ to remove the dopamine and improve the porosity; in the step S3, the direct thermal imidization treatment is carried out, when the temperature is increased to 300 ℃, dopamine is decomposed, and gaps are formed on the surface of polyimide, so that the wettability of a battery diaphragm can be improved, and the void ratio is also improved.
Preferably, the mass percentage of dopamine in the carrier in the step S1 is 5% -20%.
Preferably, in the step S2, the mass ratio of the polyimide to the dopamine-loaded carrier to the additive is 40 (1.2-10): 1-5.
Preferably, the carrier in step S1 is SiO 2 Aerogel, inorganic powder, carbon high temperature resistant material, graphite high temperature resistant material, carbon composite high temperature resistant material or fiber.
The inorganic powder is one or more selected from aluminum oxide, montmorillonite, hydrotalcite, hectorite, mica powder, kaolin, calcium carbonate, silicon dioxide or titanium dioxide.
The carbon high-temperature resistant material is selected from one or more of activated carbon, carbon black, carbon bricks or coke.
The graphite high temperature resistant material is selected from graphene and SiC-C, al 2 O 3 -C or ZrO 2 -one or more of C.
The carbon composite high temperature resistant material is selected from one or more of magnesia carbon, magnesia-calcia carbon or alumina carbon.
The fibers are selected from one or more of carbon fibers, nano-sized or micro-sized of cellulose.
Preferably, the dopamine in step S1 is one or more of dopamine hydrochloride, polydopamine, 5-hydroxy-polydopamine or polydopamine acrylamide.
Preferably, the additive in step S2 is dimethyl phthalate.
Preferably, the precursor polyamic acid PAA in step S2 is polycondensed by means of a dianhydride, a diamine in a reaction solvent.
Preferably, the molar ratio of the dianhydride to the diamine is 1:1.
Preferably, the dianhydride is selected from one or more of diphenyl sulfone tetracarboxylic dianhydride, pyromellitic dianhydride, diphenyl tetracarboxylic dianhydride or diphenyl sulfide tetracarboxylic dianhydride.
Preferably, the diamine is selected from one or more of m-phenylenediamine, p-phenylenediamine, 4 '-diaminodiphenyl ether or 4,3' -diaminodiphenyl ether.
A dopamine-modified polyimide battery separator made by the method of any one of the above.
The dopamine modified polyimide battery diaphragm is applied to a battery diaphragm and can also be used for a heat insulation film product. Because of the excellent performances of high temperature resistance, corrosion resistance, insulativity, radiation resistance and the like of the polyimide film, functional films with different purposes, high heat conductivity, high optical transparency, transparent films of optical waveguide materials and the like can be prepared, and the polyimide film can be applied to insulating layers and copper-clad plates and used in the fields of microelectronics, aviation and optical communication. It can also be used for separation membranes: a gas separation membrane, an ultrafiltration membrane, an air dehumidifying membrane, and a pervaporation membrane; for proton exchange membranes: proton exchange membrane fuel cell, direct methanol fuel cell membrane; for LB film; for special purpose composite membranes; for biological membranes; used for the anti-corrosion film; preservative film, hybrid film, chelating filter film, nonlinear optical multilayer film, microelectronic film, negative optical compensation film, gas electron multiplier film, liquid crystal vertical alignment film, etc.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through compatibility among the dopamine, the carrier, the polyimide and the additive, the dopamine is utilized to be pyrolyzed to be used as a pore-forming agent, the carrier can improve porosity and infiltration rate, or the dopamine can be utilized to increase the liquid absorption rate, so that the adhesive has a high adhesion effect, and the additive can increase connection between the carrier and the polyimide. The mutual synergistic effect of the three components not only improves the wettability of the polyimide battery diaphragm, but also improves the porosity of the battery diaphragm.
Drawings
FIG. 1 is a 5000-fold SEM image of a sample of example 1;
fig. 2 is a 5000-fold SEM image of the sample of example 2.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
The preparation methods of examples 1-16 and comparative examples 1-5 are as follows:
s1, soaking a carrier in the dopamine solution, and oscillating for 30 hours at room temperature in a water bath; obtaining a carrier loaded with dopamine;
s2, adding the dopamine-loaded carrier and the additive into the prepared precursor polyamide acid PAA solution, and fully stirring to obtain a mixed solution;
s3, coating the mixed liquid on polytetrafluoroethylene, and performing thermal imidization treatment to obtain a polyimide porous film, wherein the thermal imidization is performed according to the procedures of 100 ℃/1h, 200 ℃/1h and 300 ℃/1h, and the polyimide battery diaphragm modified by dopamine is obtained.
TABLE 1 Components and content of examples 1-16
TABLE 2 Components and contents of examples 12-16
TABLE 3 Components and contents of comparative examples 1-5
The wettability tests of the above examples and comparative examples were examined. The detection method of the infiltration performance comprises the following steps:
taking a rectangular film with the length of 10mm and the width of 10mm, placing the rectangular film in a 100mL beaker, taking 50mL of ionized water, soaking for one day, taking out, then wiping the surface of the film, weighing the water, and comparing the front and rear mass to obtain the infiltration rate and the porosity.
The formula:
porosity= (mass after soaking M 2 Mass M before soaking 1 ) /(Density of Water. Sample volume)
Infiltration rate= (mass M after soaking) 2 Mass M before soaking 1 ) Mass M before soaking 1
Table 4 wetting rate and porosity test results
| Mass M before soaking 1 /g | Mass M after soaking 2 /g | Infiltration rate (%) | Porosity (%) | |
| Example 1 | 0.083 | 0.087 | 4.81 | 1.8 |
| Example 2 | 0.051 | 0.055 | 7.84 | 2.4 |
| Example 3 | 0.043 | 0.048 | 11.62 | 3.5 |
| Comparative example 1 | 0.086 | 0.091 | 5.81 | 1.6 |
| Comparative example 5 | 0.042 | 0.043 | 2.38 | 1.4 |
Fig. 1 and 2 are SEM images of the battery separator prepared in example 1 and example 2, respectively, from which it can be seen that the pores of the surface are also more in fig. 2 than in fig. 1, which is consistent with the results of actual calculation, the porosity of example 1 is 1.8%, and the porosity of example 2 is 2.4%.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (8)
1. The preparation method of the dopamine-modified polyimide battery diaphragm is characterized by comprising the following steps of:
s1, soaking a carrier in a dopamine solution, and vibrating at room temperature until the carrier is uniformly mixed to obtain a carrier loaded with dopamine; the mass percentage of the dopamine in the carrier is 10% -20%;
s2, adding the dopamine-loaded carrier and the additive into a precursor polyamide acid PAA solution, and stirring to obtain a mixed solution, wherein the additive is one or more of polyethylene oxide, polypropylene oxide, polyethylene glycol, dimethyl phthalate, polymethyl methacrylate or polyurethane; the mass ratio of the polyamide acid to the carrier loading dopamine to the additive is 40 (1.2-10) (1-5);
s3, coating the mixed solution on polytetrafluoroethylene, and performing chemical imidization or thermal imidization treatment, wherein the thermal imidization is performed according to the program step-type heating solidification of 100 ℃/1h, 200 ℃/1h and 300 ℃/1 h.
2. The method of claim 1, wherein the carrier in step S1 is SiO 2 Aerogel, inorganic powder, carbon high temperature resistant material, graphite high temperature resistant material, carbon composite high temperature resistant material or fiber.
3. The method of claim 1, wherein the dopamine in step S1 is one or more of dopamine hydrochloride, polydopamine, 5-hydroxy-polydopamine, or polydopamine acrylamide.
4. The method of claim 1, wherein the additive in step S2 is dimethyl phthalate.
5. The method according to claim 1, wherein the precursor polyamic acid PAA in step S2 is polycondensed in a reaction solvent by means of a diamine and a dianhydride.
6. The method of claim 5, wherein the molar ratio of dianhydride to diamine is 1:1.
7. The dopamine-modified polyimide battery separator prepared by the preparation method according to any one of claims 1 to 6.
8. The use of the dopamine modified polyimide battery membrane as claimed in claim 7 in battery membranes, heat insulation membranes, separation membranes, proton exchange membranes, biological membranes.
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| CN115701440A (en) * | 2021-08-02 | 2023-02-10 | 华为技术有限公司 | Polyimide composite film, preparation method thereof and electronic equipment |
| CN113861502B (en) * | 2021-11-29 | 2022-02-25 | 国家电投集团氢能科技发展有限公司 | Preparation method of porous framework for proton exchange membrane and composite proton exchange membrane |
| CN114687000A (en) * | 2022-02-22 | 2022-07-01 | 江西师范大学 | Polydopamine @ TiO2@ PI nanofiber membrane and preparation method thereof |
| CN114824656B (en) * | 2022-05-07 | 2024-03-01 | 山东仁丰特种材料股份有限公司 | Separator paper, preparation method and battery |
| CN115347325B (en) * | 2022-09-26 | 2024-05-03 | 惠州亿纬锂能股份有限公司 | Composite diaphragm, preparation method thereof and sodium ion battery |
| CN115347326A (en) * | 2022-09-26 | 2022-11-15 | 惠州亿纬锂能股份有限公司 | Composite diaphragm, preparation method thereof and sodium ion battery |
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| CN103545474A (en) * | 2013-10-29 | 2014-01-29 | 中国第一汽车股份有限公司 | Poly-dopamine modified lithium-ion battery diaphragm and preparation method thereof |
| CN105655523A (en) * | 2016-03-31 | 2016-06-08 | 山东大学 | Deprotonated dopamine-coated film and preparation method and application thereof |
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| CN110256717A (en) * | 2019-07-03 | 2019-09-20 | 西安交通大学 | A kind of porous polyimide film and its preparation method and application |
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| CN103545474A (en) * | 2013-10-29 | 2014-01-29 | 中国第一汽车股份有限公司 | Poly-dopamine modified lithium-ion battery diaphragm and preparation method thereof |
| CN105655523A (en) * | 2016-03-31 | 2016-06-08 | 山东大学 | Deprotonated dopamine-coated film and preparation method and application thereof |
| CN108276577A (en) * | 2018-02-02 | 2018-07-13 | 天津工业大学 | Poly-dopamine modified lithium carbon nanotube graphene/polyimide composite material and preparation method thereof |
| CN110256717A (en) * | 2019-07-03 | 2019-09-20 | 西安交通大学 | A kind of porous polyimide film and its preparation method and application |
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