CN113716547B - Method for preparing negative electrode material of sodium ion battery by using waste medical mask - Google Patents
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- CN113716547B CN113716547B CN202111024725.0A CN202111024725A CN113716547B CN 113716547 B CN113716547 B CN 113716547B CN 202111024725 A CN202111024725 A CN 202111024725A CN 113716547 B CN113716547 B CN 113716547B
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention relates to the technical field of electrode materials, in particular to a method for preparing a negative electrode material of a sodium ion battery by using a waste medical mask. The invention provides a method for preparing a negative electrode material of a sodium ion battery, which comprises the following steps: mixing the waste medical mask melt-blown cloth with a sulfonation reagent to obtain a mixture; sulfonation treatment is carried out on the mixture to obtain a sulfonated product; carbonizing the sulfonated product to obtain the sodium ion battery anode material. Compared with the prior art, the technical scheme provided by the invention has the following advantages: the operation is simple, the high-pressure condition is not involved, and the large-scale recovery is convenient; the carbon yield is up to 65%; the obtained carbon material is used as a negative electrode of a sodium ion battery, shows good electrochemical performance, and realizes high-value recovery of the mask; the method provides more possibility for recycling medical waste.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a method for preparing a negative electrode material of a sodium ion battery by using a waste medical mask.
Background
At present, disposable medical masks become necessary articles for life of people, and the discarding of a large number of masks brings about environmental problems, and meanwhile, once being recycled and resold by lawless persons, the disposable medical masks can cause great threat to public health. The disposable medical mask mainly comprises a waterproof layer, a filter layer, ear bands and nose bridge strips, wherein the waterproof layer and the filter layer are made of polypropylene ultrafine fibers serving as core materials, and the proportion of the polypropylene ultrafine fibers is more than 90%. If the polypropylene can be converted into a carbon material and applied to the energy storage field, the polypropylene is certainly an effective way for high-value recycling of the disposable medical mask. If the method can realize industrialization, not only can the problem of mask recovery facing at present be solved, but also the method has guiding significance on recovery of waste surgical gowns, waste protective clothing, waste disinfection wrapping cloth and disposable sanitary cloth in the medical industry in the long term.
The lithium ion battery is the only secondary battery for commercialized application at present, and is widely applied to the fields of electronic products, electric automobiles and the like due to the advantages of small volume, light weight, high energy density, long service life and the like. But further research and application of lithium ion batteries is limited due to shortage of lithium sources and maldistribution throughout the world. Sodium ion batteries are considered to be promising alternatives to lithium ion batteries, especially in large-scale energy storage fields where energy density requirements are not high, such as new energy storage. Sodium ions are abundant in the crust, have low cost, and have similar extra-nuclear electron arrangement and electrochemical properties as lithium ions. The chemical potential (-2.71V) of sodium ions is 300mV different from that of lithium ions (-3.04V), the ionic radius is larger than that of lithium ions, and the traditional graphite negative electrode is not beneficial to intercalation and deintercalation of sodium ions due to small interlayer spacing. Therefore, the search of the anode material which is low in cost and suitable for sodium storage is a precondition for large-scale application of sodium ion batteries.
Disclosure of Invention
The invention aims to provide a method for preparing a negative electrode material of a sodium ion battery by using a waste medical mask, which not only solves the environmental problem caused by random discarding of the waste medical mask, but also can prepare the negative electrode material suitable for sodium storage.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing a negative electrode material of a sodium ion battery, which comprises the following steps:
mixing the waste medical mask melt-blown cloth with a sulfonation reagent to obtain a mixture;
sulfonation treatment is carried out on the mixture to obtain a sulfonated product;
carbonizing the sulfonated product to obtain the sodium ion battery anode material.
Preferably, the waste medical mask melt-blown cloth is replaced by other melt-blown cloth products containing polypropylene;
the other polypropylene-containing melt-blown cloth products include waste surgical gowns, waste protective clothing, waste sterilization wraps or waste disposable hygiene wraps.
Preferably, the sulphonating agent comprises concentrated sulphuric acid, oleum, sulphuryl chloride or chlorosulphonic acid;
the volume ratio of the mass of the waste medical mask melt-blown cloth to the volume of the sulfonation reagent is 1g: (10-80) mL.
Preferably, the temperature of the sulfonation treatment is 120-220 ℃ and the time is 2-24 h.
Preferably, the temperature rising rate of the sulfonation treatment to the sulfonation treatment temperature is 0.1-10 ℃/min.
Preferably, the sulfonation treatment is performed under stirring;
the stirring speed is 80-400 r/min.
Preferably, the carbonization is performed in an inert atmosphere;
the gas of the inert atmosphere is nitrogen, helium or argon.
Preferably, the carbonization temperature is 900-1400 ℃ and the time is 0.5-4 h.
Preferably, the heating rate to the carbonization temperature is 2-10 ℃/min.
The invention also provides the sodium ion battery anode material prepared by the method in the technical scheme, and the interlayer spacing of the sodium ion battery anode material is 0.374-0.392 nm.
The invention provides a method for preparing a negative electrode material of a sodium ion battery, which comprises the following steps: mixing the waste medical mask melt-blown cloth with a sulfonation reagent to obtain a mixture; sulfonation treatment is carried out on the mixture to obtain a sulfonated product; carbonizing the sulfonated product to obtain the sodium ion battery anode material. Because the mask is directly carbonized and cannot be carbonized, the invention firstly carries out sulfonation treatment on melt-blown cloth (the main component is polypropylene fiber) of the mask, so that polypropylene is dehydrogenated to form unsaturated bonds and introduce sulfonic acid groups, and then the chains react with each other to form rings, so that the molecular chains of the polypropylene fiber generate a crosslinking reaction to generate a trapezoid structure, a ring structure and a super crosslinking structure, and the heat stability is improved; meanwhile, the polypropylene fiber structure is reserved, volatile short-chain hydrocarbon is not decomposed in the subsequent high-temperature carbonization process, and the carbon forming rate is improved. In addition, small molecular gases such as sulfur dioxide and carbon dioxide are generated in the sulfonation process, and the escape of the gases plays a role in pore-forming, so that the specific surface area of the hard carbon material is improved.
The method not only realizes the recycling of the waste medical mask, but also realizes the high-value application of the product.
Compared with the prior art, the technical scheme provided by the invention has the following advantages:
1. realizing high-value recycling of the mask;
2. the carbon yield can reach 65%;
3. the obtained anode material is suitable for sodium ion batteries and has better electrochemical performance;
4. providing more possibility for recycling medical waste.
Drawings
FIG. 1 is an SEM image of a negative electrode material of a sodium ion battery of example 1;
FIG. 2 is a graph showing isothermal adsorption of the negative electrode material of the sodium ion battery according to example 1;
FIG. 3 is an XRD pattern of the negative electrode material of the sodium ion battery of example 2;
FIG. 4 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 1 at 1 st, 2 nd and 3 rd turns;
FIG. 5 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 2 at 1 st, 2 nd and 3 rd turns;
FIG. 6 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 3 at 1 st, 2 nd and 3 rd turns;
fig. 7 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 4 at 1 st, 2 nd and 3 rd turns.
Detailed Description
The invention provides a method for preparing a negative electrode material of a sodium ion battery, which comprises the following steps:
mixing the waste medical mask melt-blown cloth with a sulfonation reagent to obtain a mixture;
sulfonation treatment is carried out on the mixture to obtain a sulfonated product;
carbonizing the sulfonated product to obtain the sodium ion battery anode material.
In the present invention, all the preparation materials are commercially available products well known to those skilled in the art unless specified otherwise.
The medical mask melt-blown cloth and the sulfonating agent are mixed to obtain a mixture.
In the invention, the waste medical mask meltblown cloth is preferably replaced by other meltblown cloth products containing polypropylene; the other polypropylene-containing meltblown articles preferably include waste surgical gowns, waste protective clothing, waste sterilization wraps, or waste disposable sanitary wraps.
In the present invention, the sulfonating agent preferably includes concentrated sulfuric acid, fuming sulfuric acid, sulfuryl chloride or chlorosulfonic acid; the concentration of the concentrated sulfuric acid, fuming sulfuric acid, sulfuryl chloride or chlorosulfonic acid is not particularly limited in the present invention, and commercial concentrations well known to those skilled in the art may be used. In the invention, the sulfonating agent can enable the polypropylene fiber to remove H in the C-H bond, form unsaturated bond and introduce sulfonic acid group, and further form a ring through the mutual reaction between chains, thereby improving the thermal stability.
In the invention, the volume ratio of the mass of the waste medical mask meltblown cloth to the sulfonating agent is preferably 1g: (10-80) mL, more preferably 1g: (20-60) mL, most preferably 1g: (30-50) mL. When the waste medical mask meltblown is replaced with a waste surgical gown, a waste protective suit, a waste sterilization wrap or a waste disposable sanitary cloth, the amount of the waste surgical gown, the waste protective suit, the waste sterilization wrap or the waste disposable sanitary cloth is preferably the same as that of the waste medical mask meltblown.
The mixing is not particularly limited in this invention, and may be carried out by a process well known to those skilled in the art.
After the mixture is obtained, the mixture is subjected to sulfonation treatment to obtain a sulfonated product.
In the present invention, the temperature of the sulfonation treatment is preferably 120 to 220 ℃, more preferably 130 to 200 ℃, and most preferably 140 to 180 ℃; the time is preferably 2 to 24 hours, more preferably 5 to 20 hours, most preferably 10 to 16 hours. In the present invention, the temperature rising rate of the sulfonation to the sulfonation temperature is preferably 0.1 to 10 ℃/min, more preferably 2 to 8 ℃/min, and most preferably 4 to 6 ℃/min.
In the present invention, the sulfonation treatment is preferably performed under stirring; the stirring speed is preferably 80 to 400r/min, more preferably 100 to 300r/min, and most preferably 150 to 250r/min.
After the sulfonation treatment is completed, the present invention also preferably includes cooling, diluting, filtering, washing and drying which are sequentially performed. The cooling process is not particularly limited, and may be performed by a process well known to those skilled in the art and cooled to room temperature. In the invention, the diluent adopted for dilution is preferably deionized water, and the dilution multiple is preferably 2-10 times; in the invention, the dilution process is preferably to slowly pour the product system obtained after sulfonation into deionized water under the condition of stirring; the stirring process is not particularly limited, and may be performed by a process known to those skilled in the art. The pouring speed of the product system is not particularly limited, and the process known by the person skilled in the art is adopted to ensure that no bumping occurs. In the invention, the phenomenon that the sulfonated fiber is heated to shrink in volume can be avoided in the process, and meanwhile, the explosion boiling is avoided, so that potential safety hazards can be avoided. In the present invention, the filtration is preferably reduced pressure suction filtration; the process of the vacuum filtration is not particularly limited, and may be performed by a process known to those skilled in the art. In the invention, the washing is preferably carried out by alternately washing with deionized water and absolute ethyl alcohol in sequence; the number of times of washing is not particularly limited in the present invention, and the number of times of washing known to those skilled in the art may be used to make the object to be washed neutral. In the present invention, the drying is preferably drying, and the present invention is not limited in any particular way, and may be performed by a process well known to those skilled in the art. In the present invention, the drying is preferably performed in an oven.
After the drying is completed, the invention also preferably comprises grinding; the grinding process is not particularly limited, and may be performed by a process known to those skilled in the art.
After the sulfonated product is obtained, the sulfonated product is carbonized to obtain the sodium ion battery anode material.
In the present invention, the carbonization is preferably performed in an inert atmosphere; the gas of the inert atmosphere is preferably nitrogen, helium or argon.
In the present invention, the carbonization temperature is preferably 900 to 1400 ℃, more preferably 950 to 1350 ℃, and most preferably 1000 to 1300 ℃; the time is preferably 0.5 to 4 hours, more preferably 1 to 3 hours, most preferably 1.5 to 2.5 hours. In the present invention, the heating rate to the carbonization temperature is preferably 2 to 10 ℃/min, more preferably 3 to 8 ℃/min, and most preferably 4 to 6 ℃/min.
After the carbonization is completed, the present invention also preferably includes a post-treatment, which preferably includes cooling; the cooling process is not particularly limited, and may be performed by a process known to those skilled in the art.
In the invention, the sodium ion battery anode material is preferably hard carbon, and the interlayer spacing of the hard carbon is preferably 0.374-0.392 nm.
The method for preparing the negative electrode material of the sodium ion battery by the waste medical mask provided by the invention is described in detail below with reference to examples, but the method is not to be construed as limiting the scope of the invention.
Example 1
2g of waste medical mask melt-blown cloth is mixed with 60mL of concentrated sulfuric acid to obtain a mixture;
heating the mixture to 140 ℃ at a heating rate of 2 ℃/min, stirring at the temperature for 10 hours at a rotating speed of 200r/min, slowly pouring the obtained product system into 360mL of deionized water under the stirring condition, carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol alternately to be neutral in sequence, drying in an oven at 80 ℃ for 10 hours, and grinding to obtain a sulfonated product;
heating the sulfonated product to 1200 ℃ at a heating rate of 5 ℃/min in argon atmosphere, and preserving heat for 2 hours to carbonize to obtain the sodium ion battery anode material (0.5 g, carbon yield is 25%);
SEM test is carried out on the sodium ion battery cathode material, and the test result is shown in figure 1, and as can be seen from figure 1, the microstructure of the sodium ion battery cathode material is short fibers, the lengths are different, and the diameters are 2-10 mu m;
the sodium ion battery anode material is subjected to isothermal nitrogen adsorption test, the test result is shown in figure 2, and as can be seen from figure 2, the specific surface area of the sodium ion battery anode material is 116m 2 /g。
Example 2
2g of waste medical mask melt-blown cloth is mixed with 60mL of concentrated sulfuric acid to obtain a mixture;
heating the mixture to 150 ℃ at a heating rate of 2 ℃/min, stirring at the temperature for 10 hours at a rotating speed of 200r/min, slowly pouring the obtained product system into 360mL of deionized water under the stirring condition, carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol alternately to be neutral in sequence, drying in an oven at 80 ℃ for 10 hours, and grinding to obtain a sulfonated product;
heating the sulfonated product to 1200 ℃ at a heating rate of 5 ℃/min in argon atmosphere, and preserving heat for 2 hours to carbonize to obtain the sodium ion battery anode material (0.9 g, carbon yield is 45%);
XRD test was conducted on the negative electrode material of sodium ion battery, and the test result is shown in FIG. 3. As can be seen from FIG. 3, the interlayer spacing of the (002) crystal face of the negative electrode material of sodium ion battery is 0.379nm.
Example 3
2g of waste medical mask melt-blown cloth is mixed with 60mL of concentrated sulfuric acid to obtain a mixture;
heating the mixture to 160 ℃ at a heating rate of 2 ℃/min, stirring at the temperature for 10 hours at a rotating speed of 200r/min, slowly pouring the obtained product system into 360mL of deionized water under the stirring condition, carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol alternately to be neutral in sequence, drying in an oven at 80 ℃ for 10 hours, and grinding to obtain a sulfonated product;
and (3) heating the sulfonated product to 1200 ℃ at a heating rate of 5 ℃/min in an argon atmosphere, and preserving heat for 2 hours to carbonize to obtain the sodium ion battery anode material (1.2 g, carbon yield is 60%).
Example 4
2g of waste medical mask melt-blown cloth is mixed with 60mL of concentrated sulfuric acid to obtain a mixture;
heating the mixture to 180 ℃ at a heating rate of 2 ℃/min, stirring at the temperature for 10 hours at a rotating speed of 200r/min, slowly pouring the obtained product system into 360mL of deionized water under the stirring condition, carrying out vacuum filtration, washing with deionized water and absolute ethyl alcohol alternately to be neutral in sequence, drying in an oven at 80 ℃ for 10 hours, and grinding to obtain a sulfonated product;
and (3) heating the sulfonated product to 1200 ℃ at a heating rate of 5 ℃/min in an argon atmosphere, and preserving heat for 2 hours to carbonize to obtain the sodium ion battery anode material (1.3 g, carbon yield is 65%).
Test case
Mixing the sodium ion battery anode materials prepared in examples 1-4 with SuperP and sodium carboxymethyl cellulose respectively according to the mass ratio of 8:1:1, adding a proper amount of water, grinding into slurry, uniformly scraping the obtained slurry on a current collector copper foil, drying, and cutting into round pole pieces with the diameter of 10 mm; vacuum drying the round pole piece at 120 ℃ for 10 hours, and transferring the round pole piece into a glove box; in Ar atmosphere, sodium metal is used as a counter electrode, and 1mol of NaClO is used 4 Dissolving 1L of ethylene carbonate and diethyl carbonate solution with the volume ratio of 1:1 as electrolyte, and performing battery assembly to obtain a CR2025 button cell;
the obtained CR2025 button cell was subjected to charge and discharge test under the following conditions: the current density is 30mA/g, the discharge cut-off voltage is 0.001V, and the charge cut-off voltage is 3V;
FIG. 4 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 1 at 1 st, 2 nd and 3 rd turns; as can be seen from FIG. 4, the negative electrode material for sodium ion battery of example 1 has a reversible specific capacity of 219.7 mA.h.g -1 The first coulomb efficiency was 53%;
FIG. 5 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 2 at 1 st, 2 nd and 3 rd turns; as can be seen from FIG. 5, the embodiment2 the reversible specific capacity of the sodium ion battery anode material is 307.4mA.h.g -1 The first coulombic efficiency was 68%;
FIG. 6 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 3 at 1 st, 2 nd and 3 rd turns; as can be seen from FIG. 6, the negative electrode material for sodium ion battery of example 3 has a reversible specific capacity of 312.9mA.h.g -1 The first coulombic efficiency was 70.1%;
FIG. 7 is a charge-discharge curve of the negative electrode material of the sodium ion battery of example 4 at 1 st, 2 nd and 3 rd turns; as can be seen from FIG. 7, the negative electrode material for sodium ion battery of example 4 has a reversible specific capacity of 326.2 mA.h.g -1 The first coulombic efficiency was 69.5%.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A method for preparing a negative electrode material of a sodium ion battery, which is characterized by comprising the following steps:
mixing the waste medical mask melt-blown cloth with a sulfonation reagent to obtain a mixture;
sulfonation treatment is carried out on the mixture to obtain a sulfonated product;
carbonizing the sulfonated product to obtain the sodium ion battery anode material;
the temperature of the sulfonation treatment is 160-220 ℃.
2. The method of claim 1 wherein said spent medical mask meltblown is replaced with another polypropylene-containing meltblown article;
the other polypropylene-containing melt-blown cloth products include waste surgical gowns, waste protective clothing, waste sterilization wraps or waste disposable hygiene wraps.
3. The method of claim 1 or 2, wherein the sulfonating agent comprises concentrated sulfuric acid, fuming sulfuric acid, sulfuryl chloride or chlorosulfonic acid;
the volume ratio of the mass of the waste medical mask melt-blown cloth to the volume of the sulfonation reagent is 1g: (10-80) mL.
4. The method according to claim 1 or 2, wherein the sulfonation is for 2 to 24 hours.
5. The method according to claim 1, wherein a temperature rising rate of the sulfonation treatment to the sulfonation treatment is 0.1 to 10 ℃/min.
6. The method of claim 5, wherein the sulfonation is performed under stirring;
the stirring speed is 80-400 r/min.
7. The method according to claim 1 or 2, wherein the carbonization is performed in an inert atmosphere;
the gas of the inert atmosphere is nitrogen, helium or argon.
8. The method according to claim 1 or 2, wherein the carbonization temperature is 900-1400 ℃ and the time is 0.5-4 hours.
9. The method of claim 8, wherein the rate of heating to the carbonization temperature is 2-10 ℃/min.
10. The negative electrode material of the sodium ion battery prepared by the method of any one of claims 1-9, wherein the interlayer spacing of the negative electrode material of the sodium ion battery is 0.374-0.390 nm.
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