CN114014354B - Method for preparing nano tin dioxide @ nitrogen-doped carbon composite material and application - Google Patents

Method for preparing nano tin dioxide @ nitrogen-doped carbon composite material and application Download PDF

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CN114014354B
CN114014354B CN202111255275.6A CN202111255275A CN114014354B CN 114014354 B CN114014354 B CN 114014354B CN 202111255275 A CN202111255275 A CN 202111255275A CN 114014354 B CN114014354 B CN 114014354B
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nitrogen
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tin dioxide
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周颖
李官书
王春雷
方涛
张赛
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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    • H01M4/625—Carbon or graphite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01P2004/00—Particle morphology
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    • C—CHEMISTRY; METALLURGY
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a method for preparing a nano tin dioxide @ nitrogen-doped carbon composite material and application thereof, and belongs to the technical field of material preparation. The method comprises the following steps: adding coal or petroleum heavy organic matters, nitrobenzene, anhydrous tin tetrachloride and a solvent into a reactor, and reacting for a certain time under certain conditions; and after the reaction is finished, adding a washing solution into the reaction system, and filtering, washing and drying the mixture to obtain a product A. And carbonizing the product A in an inert atmosphere to obtain the nano tin dioxide @ nitrogen-doped carbon composite material. The preparation method has the advantages of low cost, simple process, short reaction time, environmental protection, energy conservation, convenient operation and large-scale preparation, and the prepared composite material can be used as a battery cathode material.

Description

Method for preparing nano tin dioxide @ nitrogen-doped carbon composite material and application
Technical Field
The invention relates to the technical field of material preparation, in particular to a method for preparing a nano tin dioxide @ nitrogen-doped carbon composite material by one-pot boiling and low-temperature carbonization.
Background
With the rapid development of electric vehicles and new energy technologies, the demand for energy supply and storage devices having high energy density and power density is more urgent. Compared with the commercial graphite which has a lithium storage theoretical capacity of only 382mAh/g, the conversion type negative electrode material tin dioxide is widely researched by scholars due to the advantages of high specific capacity, low price, easy obtaining and environmental friendliness. However, tin dioxide has the disadvantages of significant volume expansion effect and poor electrical conductivity, and thus needs to be compounded with carbon materials to make up for the deficiency. The introduction of nitrogen into the carbon layer can improve the conductivity and lithium storage capacity of the carbon layer, so that the electrochemical performance of the tin dioxide @ nitrogen doped carbon composite material is further improved.
CN109768269A discloses a nitrogen-sulfur double-doped porous carbon-coated tin dioxide composite material and a preparation method thereof, phenolic resin is used as a carbon source, 2,5-dimercapto-1,3,4-thiadiazole is used as a sulfur source and a nitrogen source, tin dioxide is coated, and the prepared cathode material has an N-S doped carbon layer. CN108123126A discloses a preparation method of a high-capacity lithium ion battery tin dioxide/nitrogen-doped graphene composite negative electrode material, which comprises the steps of firstly carrying out hydrothermal reaction on graphene oxide with a certain concentration and a solution containing a nitrogen source to obtain a three-dimensional nitrogen-doped graphene sponge, carrying out hydrothermal reaction again to load tin dioxide, and calcining to obtain the composite material which has a three-dimensional nitrogen-containing conductive network structure and is loaded with nano tin dioxide. CN108321376A discloses a nitrogen-doped porous carbon nanofiber @ tin dioxide lithium ion battery cathode material and a preparation method thereof, the nanofiber containing ZIF-8 is prepared by an electrostatic spinning method, a layer of tin dioxide nanoparticles is coated by a hydrothermal method after high-temperature calcination, and finally a layer of polypyrrole is coated and calcined at high temperature. The methods all need to prepare the nitrogen-doped carbon matrix and the nano tin dioxide respectively, and have the problems of complex flow, expensive raw materials, difficulty in large-scale preparation and great environmental pollution.
Disclosure of Invention
Aiming at the problems that the raw materials for preparing the nano tin dioxide @ nitrogen-doped carbon composite material in the prior art are expensive, the preparation process is complex and large-scale preparation is difficult, the invention provides a method for preparing the nano tin dioxide @ nitrogen-doped carbon composite material by a one-pot method and low-temperature carbonization. The preparation method comprises the steps of taking coal or petroleum heavy organic matters and nitrobenzene as raw materials, obtaining a nano tin dioxide @ polyarylamine composite material through a polymerization reaction under the catalysis of anhydrous tin tetrachloride, and carbonizing an obtained product at a low temperature to obtain the nano tin dioxide @ nitrogen-doped carbon composite material. To increase the degree of polymerization, a crosslinking agent may be added to the initial reaction mixture.
The invention provides a method for preparing a nano tin dioxide @ nitrogen-doped carbon composite material, which comprises the following steps:
adding coal or petroleum heavy organic matters, nitrobenzene, anhydrous stannic chloride and a solvent into a reactor, reacting for a certain time under a certain condition, adding a washing solution into the reaction system, and filtering, washing and drying the obtained mixture to obtain a product A; and carbonizing the product A in an inert atmosphere to obtain the nano tin dioxide @ nitrogen-doped carbon composite material.
The polymerization degree can be improved by adding a cross-linking agent while adding the coal or petroleum heavy organic matter, nitrobenzene, anhydrous stannic chloride and solvent into the reactor.
The coal or petroleum heavy organic matter is coal tar and one of distillate oil (phenol oil, naphthalene oil, washing oil, anthracene oil and anthracene oil), atmospheric and vacuum residue, ethylene tar, coal direct liquefaction asphalt, coal asphalt or petroleum asphalt.
The cross-linking agent is one of dimethoxymethane, oxalyl chloride, chloroform or carbon tetrachloride.
The solvent is one of nitrobenzene, dichlorobenzene, trichlorobenzene and p-dichlorobenzene.
The mass ratio of the coal or petroleum heavy organic matters to the nitrobenzene is 1:0.1 to 100.
The mass ratio of the coal or petroleum heavy organic matter to the cross-linking agent is 1:0 to 10.
The mass ratio of the coal or petroleum heavy organic matter to the anhydrous stannic chloride is 1:1 to 30.
The mass ratio of the coal or petroleum heavy organic matters to the solvent is 1:5 to 100; the reaction temperature is 100-300 ℃, and the reaction time is 0.5-30h.
The washing solution is selected from one of water, ethanol, ammonia water, naOH solution and KOH solution, wherein the concentration of the alkali liquor of the ammonia water, the NaOH solution or the KOH solution is 5-30wt.%, and the pH of the solution after reaction is ensured to be 8-12 after the ammonia water, the NaOH solution or the KOH solution is added; the solvent used for washing after filtration is one or more of water, methanol and ethanol.
The drying temperature is 60-350 ℃, and the drying time is 6-48 h; the carbonization temperature is 400-900 ℃, the carbonization time is 0.5-5 h, and the inert atmosphere is nitrogen or argon.
The content of the tin dioxide of the nano tin dioxide @ nitrogen-doped carbon composite material is 10-90 wt.%, and the particle size is 2-50 nm; the nitrogen content is 0.5-20 wt.%.
The nano tin dioxide @ nitrogen doped carbon composite material is applied to lithium ion and sodium ion batteries.
The invention has the beneficial effects that: the method has the advantages of low cost, simple flow, short reaction time, environmental protection, energy conservation, easy operation and large-scale preparation, and the obtained product has better battery cathode performance and can be prepared on a large scale. The method provides a new technology for the low-cost rapid preparation of the nano tin dioxide @ nitrogen-doped carbon composite material, and realizes the high value-added utilization of heavy organic matters.
Drawings
FIG. 1 is XRD patterns of the materials of examples 1-4, wherein (a) is an XRD pattern before carbonization of the composite material, and (b) is an XRD pattern after carbonization of the composite material.
FIG. 2 is the thermogravimetric curves of the materials of examples 1-4.
Fig. 3 shows the lithium battery performance of the material in application example 1, wherein (a) shows the lithium battery rate performance of the material in application example 1, and (b) shows the lithium battery cycle performance of the material in application example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited thereto.
Example 1
2.5g of nitrobenzene, 1.5g of petroleum pitch, 11g of anhydrous tin tetrachloride and 14.7g of p-dichlorobenzene were charged into a 50mL single-neck flask. Stirring and refluxing for 5h in an oil bath at 200 ℃, diluting the reaction solution with ethanol, filtering, washing the obtained solid with ethanol and water for 3 times respectively, drying in an oven at 80 ℃ for 24h, and marking the sample as NB-PP-2.5. And finally, carbonizing the sample at 500 ℃ for 3h under an argon atmosphere to obtain the negative electrode material NB-PP-2.5 for 1.5-500-3h.
Example 2
2.5g of nitrobenzene, 1.5g of petroleum pitch, 11g of anhydrous tin tetrachloride, 3g of dimethoxymethane and 14.7g of p-dichlorobenzene were charged into a 50mL single-neck flask. Stirring and refluxing the mixture in an oil bath at 200 ℃ for 5 hours, diluting the reaction solution with ethanol, filtering, washing the obtained solid with ethanol and water for 3 times respectively, drying the solid in an oven at 80 ℃ for 24 hours, and marking the sample as NB-PP-FDA-2.5. And finally, carbonizing the sample at 500 ℃ for 3h under an argon atmosphere to obtain the anode material NB-PP-FDA-2.5.
Table 1 compositions of samples in examples 1 and 2
Figure BDA0003323897310000031
* : the contents of the elements other than C, N, H were calculated by the elemental analysis result subtraction method.
* *: sn content converted from thermogravimetric analysis results.
Example 3
10g of nitrobenzene, 1.5g of petroleum pitch, 11g of anhydrous tin tetrachloride, 3g of dimethoxymethane and 14.7g of p-dichlorobenzene were charged into a 50mL single-neck flask. Stirring and refluxing the mixture in an oil bath at 200 ℃ for 5 hours, diluting the reaction solution with ethanol, filtering, washing the obtained solid with ethanol and water respectively for 3 times, and drying the solid in an oven at 80 ℃ for 24 hours, wherein the sample is marked as NB-PP-FDA-10. Finally, carbonizing the sample at 500 ℃ for 3h under an argon atmosphere to obtain the negative electrode material NB-PP-FDA-10 for 3-500-3h.
Example 4
2.5g of nitrobenzene, 1.5g of petroleum pitch, 11g of anhydrous tin tetrachloride, 3g of dimethoxymethane and 14.7g of p-dichlorobenzene were charged into a 50mL single-neck flask. Stirring and refluxing the mixture in an oil bath at 200 ℃ for 5 hours, adding 12mL of 25wt.% concentrated ammonia water into the reaction solution, stirring and filtering, washing the obtained solid with ethanol and water for 3 times respectively, and drying the solid in an oven at 80 ℃ for 24 hours, wherein the sample is marked as NB-PP-FDA-2.5. And finally, carbonizing the sample at 500 ℃ for 3h under an argon atmosphere to obtain a negative electrode material NB-PP-FDA-2.5.
Example 5
50mL of nitrobenzene, 1.5g of naphthalene oil, and 11g of anhydrous tin tetrachloride were charged into a 100mL single-neck flask. Stirring and refluxing the mixture in an oil bath at the temperature of 200 ℃ for reaction for 2 hours, adding 12mL25wt.% concentrated ammonia water into the reaction solution, stirring and filtering the mixture, washing the obtained solid with ethanol and water for 3 times respectively, and drying the solid in an oven at the temperature of 80 ℃ for 24 hours. And finally, carbonizing the sample at 500 ℃ for 3h in an argon atmosphere to obtain the cathode material. In this example, nitrobenzene is both a reactant and acts as a solvent.
Example 6
50mL of nitrobenzene, 1.5g of wash oil, and 11g of anhydrous tin tetrachloride were charged into a 100mL single-neck flask. Stirring and refluxing the mixture in an oil bath at the temperature of 200 ℃ for reaction for 2 hours, adding 12mL25wt.% concentrated ammonia water into the reaction solution, stirring and filtering the mixture, washing the obtained solid with ethanol and water for 3 times respectively, and drying the solid in an oven at the temperature of 80 ℃ for 24 hours. And finally, carbonizing the sample at 500 ℃ for 3h in an argon atmosphere to obtain the cathode material. In this example, nitrobenzene is both a reactant and acts as a solvent.
Application example 1
The samples of examples 1 to 4, acetylene black and polyvinylidene fluoride were mixed in a mass ratio of 8. Using 1M LiPF 6 DEC = 1vol.%, a mixed solution with 10wt.% FEC added as an electrolyte, and a Celgard2400 polypropylene PP film as a separator. The battery is in the absence of water and oxygen (O) 2 <0.1ppm，H 2 O<0.1 ppm) was assembled in a glove box. The rate performance and cycle performance were tested on LAND CT 2001A.
It can be seen from table 1 that the nitrogen element was successfully introduced into the carbon matrix. From fig. 1, it can be seen that the XRD spectrum corresponding to the prepared material contains a broad diffraction peak of the nano tin dioxide particles. From FIG. 2, it can be seen that the content of nano tin dioxide in the composite material can be increased by increasing the amount of the cross-linking agent and washing the reaction solution with the alkali solution. As can be seen from (a) in FIG. 3, 1.5 to 500-3h of NB-PP-FDA-2.5 has specific capacities of 626.4mAh/g, 492.1mAh/g, 403.0mAh/g, 363.4mAh/g, 303.1mAh/g and 233.7mAh/g at current densities of 0.1A/g, 0.2A/g, 0.5A/g, 1A/g, 2A/g and 5A/g, respectively, and is obviously improved compared with 1.5 to 500-3h of a sample NB-PP-2.5 without the crosslinking agent. As can be seen from (b) in FIG. 3, the capacity increased to 531.7mAh/g after 500 cycles of NB-PP-FDA-2.5 for 1.5. In general, the prepared nano tin dioxide @ nitrogen doped carbon composite material has excellent electrochemical performance when used as a lithium ion battery cathode material.
Application example 2
The samples of examples 1 to 4, acetylene black and polyvinylidene fluoride were mixed in a mass ratio of 8. With 1M NaClO 4 DEC =1, and Whatman GF/D glass fiber is a diaphragm. The battery is in the absence of water and oxygen (O) 2 <0.1ppm，H 2 O<0.1 ppm) was assembled in a glove box. The rate performance and cycle performance were tested on LAND CT 2001A.

Claims (9)

1. A method for preparing a nano tin dioxide @ nitrogen-doped carbon composite material is characterized by comprising the following steps:
the tin-containing nitrogen-containing polymer carbon precursor A is synthesized by the solution polymerization reaction of heavy organic matters and nitrobenzene catalyzed by anhydrous stannic chloride, and specifically comprises the following steps: adding coal or petroleum heavy organic matters, nitrobenzene, anhydrous stannic chloride and a solvent into a reactor, reacting at 100-300 ℃ for 0.5-30h, adding a washing solution into the reaction system, filtering, washing and drying the obtained mixture to obtain a product A; and carbonizing the product A in an inert atmosphere to obtain the nano tin dioxide @ nitrogen-doped carbon composite material.
2. The method for preparing nano tin dioxide @ nitrogen-doped carbon composite material according to claim 1, wherein a cross-linking agent can be added to improve the polymerization degree, tin content and lithium storage capacity while adding coal or petroleum heavy organics, nitrobenzene, anhydrous tin tetrachloride and a solvent into a reactor.
3. The method for preparing nano tin dioxide @ nitrogen doped carbon composite material as claimed in claim 2, wherein: the coal or petroleum heavy organic matter is one of coal tar and distillate oil thereof, atmospheric and vacuum residue, ethylene tar, coal directly liquefied asphalt, coal asphalt or petroleum asphalt; the cross-linking agent is one of dimethoxymethane, oxalyl chloride, chloroform or carbon tetrachloride; the solvent is one of nitrobenzene, dichlorobenzene, trichlorobenzene and paradichlorobenzene; the mass ratio of the coal or petroleum heavy organic matters to the nitrobenzene is 1:0.1 to 100; the mass ratio of the coal or petroleum heavy organic matter to the cross-linking agent is 1:0 to 10, the mass ratio of the coal or petroleum heavy organic matter to the anhydrous stannic chloride is 1:1 to 30; the mass ratio of the coal or petroleum heavy organic matter to the solvent is 1:5 to 100.
4. The method of preparing nano tin dioxide @ nitrogen doped carbon composite material as claimed in claim 1, 2 or 3, wherein: coal tar distillate oil in the coal or petroleum series heavy organic matters is phenol oil, naphthalene oil, washing oil, anthracene oil or anthracene oil, the washing oil is selected from one of water, ethanol, ammonia water, naOH solution and KOH solution, wherein the alkali liquor concentration of the ammonia water, the NaOH solution or the KOH solution is 5-30wt.%, and the pH of the solution after reaction is ensured to be 8-12 after the ammonia water, the NaOH solution or the KOH solution is added; the solvent used for washing after filtration is one or more of water, methanol and ethanol.
5. The method of preparing nano tin dioxide @ nitrogen doped carbon composite material as claimed in claim 1, 2 or 3, wherein: the drying temperature is 60-350 ℃, and the drying time is 6-48 h; the carbonization temperature is 400-900 ℃, the carbonization time is 0.5-5 h, and the inert atmosphere is nitrogen or argon.
6. The method of preparing nano tin dioxide @ nitrogen doped carbon composite material as claimed in claim 4, wherein: the drying temperature is 60-350 ℃, and the drying time is 6-48 h; the carbonization temperature is 400-900 ℃, the carbonization time is 0.5-5 h, and the inert atmosphere is nitrogen or argon.
7. The method for preparing nano tin dioxide @ nitrogen doped carbon composite material as claimed in claim 1, 2, 3 or 6, wherein: the content of tin dioxide in the nano tin dioxide @ nitrogen-doped carbon composite material is 10-90 wt.%, and the particle size is 2-50 nm; the nitrogen content is 0.5-20 wt.%.
8. The method of preparing nano tin dioxide @ nitrogen-doped carbon composite material as claimed in claim 5, wherein: the content of tin dioxide in the nano tin dioxide @ nitrogen-doped carbon composite material is 10-90 wt.%, and the particle size is 2-50 nm; the nitrogen content is 0.5-20 wt.%.
9. The application of the nano tin dioxide @ nitrogen-doped carbon composite material prepared by the method of any one of claims 1 to 8 in lithium ion and sodium ion batteries.
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