CN110615436A - Method for preparing N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues - Google Patents
Method for preparing N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues Download PDFInfo
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Abstract
The invention discloses a method for preparing an N-doped porous carbon composite lithium battery cathode material by utilizing coal humic acid extraction residues, which takes red-peak lignite with lower ash content as a raw material, and the brown coal is crushed into powder, cleaned and dried in the sun; separating the lignite raw material into residues and an extracting solution by taking KOH and urea as a composite extracting agent; and (2) activating and remolding the pore channel of the extracted residue by using KOH as an activating agent and urea as a nitrogen source through a chemical activation method, and performing nitrogen doping modification on the porous carbon by using urea as the nitrogen source to prepare the N-doped porous carbon composite lithium battery cathode material with controllable components and structure.
Description
Technical Field
The invention relates to the field of negative electrode materials of N-doped porous carbon composite lithium batteries, in particular to a method for preparing the negative electrode material of the N-doped porous carbon composite lithium battery by utilizing coal humic acid extraction residues.
Background
Lignite resources in China are rich, and reserves account for more than 55% of the total reserves of coal; the storage amount of lignite in the inner Mongolia autonomous region is the largest, and accounts for 77% of the national lignite resource amount; wherein, the content of total humic acid in the inner Mongolia red peak lignite is 31.6 percent, the content of free humic acid is 24.9 percent, the content of ash is 14.53 percent, and the content of water is 27.8 percent; the humic acid is mainly an organic high molecular polymer formed and accumulated by animal and plant remains through microbial decomposition, conversion and a series of geophysical and chemical reactions, has water solubility, and is widely present in carbonaceous sedimentary rocks such as water, soil, peat, lignite, weathered coal, shale and the like; the humic acid structure contains rich active oxygen-containing functional groups such as carboxyl, phenolic hydroxyl, carbonyl, sulfonic group, methoxy group and the like, and has important influence on the acidity, ion exchange property, colloid property and complexing property; the method is widely applied to various fields of agriculture, forestry, pasture, petroleum, chemical industry, building materials, medicine, health, environmental protection and the like; particularly, ecological agricultural construction, pollution-free agricultural production, green food, pollution-free and environment-friendly properties and the like are advocated at present, and the humic acid is more advocated; lignite contains rich humic acid and is a main resource for utilizing the humic acid on a large scale; compared with soil humic acid, the lignite humic acid has higher carbon content, lower nitrogen content and higher hydrogen content, and shows that the chemical activity and the substitution performance are better; researchers at home and abroad extract humic acid in lignite by using an alkali solution acid precipitation method, an acid extraction agent method, a microorganism dissolution method and the like, and the extraction rate of the humic acid reaches more than 80 percent; at least more than 25% of organic matters in the residue after the humic acid is extracted are not fully utilized; if the organic matters are carbonized and activated to prepare the N-doped porous carbon composite lithium battery cathode material, the method has great significance for realizing the clean, efficient and high-added-value utilization of the lignite; at present, the prior art has not been researched and reported in this respect.
Disclosure of Invention
The invention aims to provide a method for preparing an N-doped porous carbon composite lithium battery cathode material by utilizing coal humic acid extraction residues, which takes the akage lignite with lower ash content as a raw material, pulverizes the akage lignite into powder, cleans the powdered akage lignite, and dries the lignite; separating the lignite raw material into residues and an extracting solution by taking KOH and urea as a composite extracting agent; and (2) activating and remolding the pore channel of the extracted residue by using KOH as an activating agent and urea as a nitrogen source through a chemical activation method, and performing nitrogen doping modification on the porous carbon by using urea as the nitrogen source to prepare the N-doped porous carbon composite lithium battery cathode material with controllable components and structure.
The technical scheme adopted by the invention is as follows: a method for preparing an N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues comprises the following steps:
s1: preparing a lignite raw material: pulverizing lignite into powder, cleaning the powder by using distilled water, and drying the powder in the sun to prepare a clean lignite raw material;
s2: alkali extraction of KOH and urea: weighing the clean lignite raw material obtained by the processing of the step S1, and mixing the clean lignite raw material with urea, wherein the mass ratio of the lignite raw material to the urea is 1: 0.5-1: 2; mixing the mixture with a KOH solution to prepare a mixture, wherein the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 5-1: 30; the mass fraction of the KOH solution is 1 to 3 percent; then, preserving the heat of the prepared solid-liquid mixture in a water bath at the temperature of 70-100 ℃ for 70-100 min; taking out, cooling, stirring with a magnetic stirrer for reaction, centrifuging with a centrifuge, and separating to obtain residue and extractive solution;
s3: putting the residue obtained in the step S2 into a tubular furnace with nitrogen as protective gas, and carbonizing and activating at the temperature of 410-720 ℃ for 0.4-2.2 h to obtain a carbonized and activated product;
s4: soaking the carbonized and activated product prepared in the step S3 in a hydrochloric acid solution, performing suction filtration, washing with deionized water, and drying in a forced air drying oven to obtain the N-doped porous carbon composite lithium battery cathode material; the concentration of the hydrochloric acid solution is 0.2-2.5 mol/L.
Further, the brown coal used in the step S1 is brown coal in the inner mongolian red peak region.
Further, in a preferred embodiment, in step S2, the mass ratio of the raw lignite material to the urea is 1: 1; the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 20; the mass fraction of the KOH solution is 2 percent; then, the prepared solid-liquid mixture is kept for 90min in a water bath with the temperature of 90 ℃;
in step S3: carbonizing and activating for 1h at the temperature of 600 ℃ to obtain a carbonized and activated product;
in step S4: the concentration of the hydrochloric acid solution used was 1.0 mol/L.
The invention has the beneficial effects that: the invention provides a method for preparing an N-doped porous carbon composite lithium battery cathode material by utilizing coal humic acid extraction residues, which takes red-peak lignite with lower ash content as a raw material, pulverizes the brown coal into powder, cleans the brown coal, and dries the brown coal; separating the lignite raw material into residues and an extracting solution by taking KOH and urea as a composite extracting agent; and (2) activating and remolding the pore channel of the extracted residue by using KOH as an activating agent and urea as a nitrogen source through a chemical activation method, and performing nitrogen doping modification on the porous carbon by using urea as the nitrogen source to prepare the N-doped porous carbon composite lithium battery cathode material with controllable components and structure.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Fig. 2 is a diagram of isothermal adsorption and desorption (BET) of the negative electrode material of the N-doped porous carbon composite lithium battery prepared by the method in example 1.
Fig. 3 is a cycle performance diagram of the negative electrode material of the N-doped porous carbon composite lithium battery prepared by the method in embodiment 1 of the invention.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and examples, which are set forth below for illustrating the technical solutions of the present invention only and are not limited thereto.
A method for preparing an N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues is shown in a process flow of figure 1, and comprises the following steps:
s1: preparing a lignite raw material: pulverizing lignite into powder, cleaning the powder by using distilled water, and drying the powder in the sun to prepare a clean lignite raw material; the lignite used in the method of the invention is preferably lignite in the red peak area of inner Mongolia; impurities mixed in the lignite and silt on the surface can be removed by repeatedly cleaning the lignite with distilled water;
s2: alkali extraction of KOH and urea: weighing the clean lignite raw material obtained by the processing of the step S1, and mixing the clean lignite raw material with urea, wherein the mass ratio of the lignite raw material to the urea is 1: 0.5-1: 2; mixing the mixture with a KOH solution to prepare a mixture, wherein the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 5-1: 30; the mass fraction of the KOH solution is 1 to 3 percent; then, preserving the heat of the prepared solid-liquid mixture in a water bath at the temperature of 70-100 ℃ for 70-100 min; taking out, cooling, stirring with a magnetic stirrer for reaction, centrifuging with a centrifuge, and separating to obtain residue and extractive solution; after the treatment of the step, humic acid is separated from the lignite particles and dissolved in the extracting solution, porous holes are formed on the surfaces of the lignite particles, the specific surface area of the lignite particles is increased, the residues have certain adsorption capacity, and the holes on the surfaces provide embeddable regions for adsorbed ions;
s3: putting the residue obtained in the step S2 into a tubular furnace with nitrogen as protective gas, and carbonizing and activating at the temperature of 410-720 ℃ for 0.4-2.2 h to obtain a carbonized and activated product;
s4: soaking the carbonized and activated product prepared in the step S3 in a hydrochloric acid solution, performing suction filtration, washing with deionized water, and drying in a forced air drying oven to obtain the N-doped porous carbon composite lithium battery cathode material; the concentration of the hydrochloric acid solution is 0.2-2.5 mol/L.
The method takes the red peak lignite with lower ash content as a raw material, and the brown lignite is crushed into powder, cleaned and dried; separating the lignite raw material into residues and an extracting solution by taking KOH and urea as a composite extracting agent; the extracting solution separated in the step S2 can be used for preparing humic acid, because the invention mainly solves the problems that how to prepare the negative electrode material of the N-doped porous carbon composite lithium battery by using the residue and how to prepare the humic acid by using the extracting solution separated in the step S2 are not described in detail in the patent application of the specific preparation process; and (2) activating and remolding the pore channel of the extracted residue by using KOH as an activating agent and urea as a nitrogen source through a chemical activation method, and performing nitrogen doping modification on the porous carbon by using urea as the nitrogen source to prepare the N-doped porous carbon composite lithium battery cathode material with controllable components and structure.
The invention is further illustrated below with reference to specific examples. It is to be understood, however, that these examples are illustrative only and are not to be construed as limiting the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the manufacturer.
Example 1
S1: preparing a lignite raw material: pulverizing the red brown coal into powder, cleaning with distilled water, and sun drying to obtain clean brown coal raw material;
s2: alkali extraction of KOH and urea: weighing the clean lignite raw material obtained by the step S1, and mixing the clean lignite raw material with urea, wherein the mass ratio of the lignite raw material to the urea is 1: 1; mixing the mixture with a KOH solution to prepare a mixture, wherein the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 20; the mass fraction of the KOH solution is 2 percent; then, the prepared solid-liquid mixture is kept for 90min in a water bath with the temperature of 90 ℃; taking out, cooling, stirring with a magnetic stirrer for reaction, centrifuging with a centrifuge, and separating to obtain residue and extractive solution;
s3: putting the residue obtained in the step S2 into a tubular furnace with nitrogen as protective gas, and carbonizing and activating for 1h at the temperature of 600 ℃ to obtain a carbonized and activated product;
s4: soaking the carbonized and activated product prepared in the step S3 in a hydrochloric acid solution, performing suction filtration, washing with deionized water, and drying in a forced air drying oven to obtain the N-doped porous carbon composite lithium battery cathode material; the concentration of the hydrochloric acid solution was 1.0 mol/L.
As shown in fig. 2, which is a graph of isothermal desorption (BET) of the negative electrode material of the N-doped porous carbon composite lithium battery prepared in this example, it can be seen from the graph (a) that an inflection point B exists in a low relative pressure (P/P0) region on the N2 desorption isotherm of the sample; in addition, when P/P0= 0.4-0.9, an H4 hysteresis loop appears on the isothermal curve of the sample, because capillary condensation occurs in the adsorption process of the sample, and the isothermal curve obtained in the desorption process does not coincide with the isothermal curve obtained in the adsorption process; according to IUPAC classification, the absorption and desorption curve of the sample is an IV-type isotherm, which indicates that the material has a mesoporous structure; from the curve of the graph (b), the pore diameter distribution of the material can be seen to be mesoporous and microporous; the pore structures can relieve the volume expansion of lithium ions during the de-intercalation and the intercalation and prevent pulverization; the lithium storage sites of the material can be increased, and the specific capacity of the material can be increased.
Fig. 3 is a graph showing the cycle performance of the negative electrode material of the N-doped porous carbon composite lithium battery prepared by the method in example 1 of the present invention; the traditional graphite lithium battery cathode only has the specific capacity of 375mA/g, while the specific capacity of the material prepared by the embodiment reaches 1072mA/g, which is nearly 3 times of that of the existing graphite lithium battery cathode.
Example 2
S1: preparing a lignite raw material: pulverizing the red brown coal into powder, cleaning with distilled water, and sun drying to obtain clean brown coal raw material;
s2: alkali extraction of KOH and urea: weighing the clean lignite raw material obtained by the step S1, and mixing the clean lignite raw material with urea, wherein the mass ratio of the lignite raw material to the urea is 1: 0.5; mixing the mixture with a KOH solution to prepare a mixture, wherein the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 5; the mass fraction of the KOH solution is 1 percent; then, the prepared solid-liquid mixture is kept warm for 70min in a water bath with the temperature of 70 ℃; taking out, cooling, stirring with a magnetic stirrer for reaction, centrifuging with a centrifuge, and separating to obtain residue and extractive solution;
s3: putting the residue obtained in the step S2 into a tubular furnace with nitrogen as protective gas, and carbonizing and activating for 0.4h at the temperature of 410 ℃ to obtain a carbonized and activated product;
s4: soaking the carbonized and activated product prepared in the step S3 in a hydrochloric acid solution, performing suction filtration, washing with deionized water, and drying in a forced air drying oven to obtain the N-doped porous carbon composite lithium battery cathode material; the concentration of the hydrochloric acid solution was 0.2 mol/L.
Example 3
S1: preparing a lignite raw material: pulverizing the red brown coal into powder, cleaning with distilled water, and sun drying to obtain clean brown coal raw material;
s2: alkali extraction of KOH and urea: weighing the clean lignite raw material obtained by the step S1, and mixing the clean lignite raw material with urea, wherein the mass ratio of the lignite raw material to the urea is 1: 2; mixing the mixture with a KOH solution to prepare a mixture, wherein the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 30; the mass fraction of the KOH solution is 3 percent; then, the prepared solid-liquid mixture is kept for 100min in a water bath with the temperature of 100 ℃; taking out, cooling, stirring with a magnetic stirrer for reaction, centrifuging with a centrifuge, and separating to obtain residue and extractive solution;
s3: putting the residue obtained in the step S2 into a tubular furnace with nitrogen as protective gas, and carrying out carbonization and activation for 2.2h at the temperature of 720 ℃ to obtain a carbonization and activation product;
s4: soaking the carbonized and activated product prepared in the step S3 in a hydrochloric acid solution, performing suction filtration, washing with deionized water, and drying in a forced air drying oven to obtain the N-doped porous carbon composite lithium battery cathode material; the concentration of the hydrochloric acid solution was 2.5 mol/L.
In the above examples, example 1 was the most preferable example obtained by comparative experiments, in which the extraction rate of humic acid was the largest in the experiments, so that more pores were formed on the surface of the lignite particles and the specific capacity was also the largest in the experiments.
Although the present invention has been described in detail with reference to the foregoing examples, it will be apparent to one skilled in the art that various changes in the embodiments and/or modifications of the embodiments and/or portions thereof may be made, and all changes, equivalents, and modifications that fall within the spirit and scope of the invention are therefore intended to be embraced by the appended claims.
Claims (3)
1. The method for preparing the N-doped porous carbon composite lithium battery cathode material by using the coal humic acid extraction residues is characterized by comprising the following steps of:
s1: preparing a lignite raw material: pulverizing lignite into powder, cleaning the powder by using distilled water, and drying the powder in the sun to prepare a clean lignite raw material;
s2: alkali extraction of KOH and urea: weighing the clean lignite raw material obtained by the processing of the step S1, and mixing the clean lignite raw material with urea, wherein the mass ratio of the lignite raw material to the urea is 1: 0.5-1: 2; mixing the mixture with a KOH solution to prepare a mixture, wherein the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 5-1: 30; the mass fraction of the KOH solution is 1 to 3 percent; then, preserving the heat of the prepared solid-liquid mixture in a water bath at the temperature of 70-100 ℃ for 70-100 min; taking out, cooling, stirring with a magnetic stirrer for reaction, centrifuging with a centrifuge, and separating to obtain residue and extractive solution;
s3: putting the residue obtained in the step S2 into a tubular furnace with nitrogen as protective gas, and carbonizing and activating at the temperature of 410-720 ℃ for 0.4-2.2 h to obtain a carbonized and activated product;
s4: soaking the carbonized and activated product prepared in the step S3 in a hydrochloric acid solution, performing suction filtration, washing with deionized water, and drying in a forced air drying oven to obtain the N-doped porous carbon composite lithium battery cathode material; the concentration of the hydrochloric acid solution is 0.2-2.5 mol/L.
2. The method for preparing the N-doped porous carbon composite lithium battery anode material by using the coal humic acid extraction residues as claimed in claim 1, which is characterized in that: the lignite used in the step S1 is lignite in the red peak area of inner mongolian city.
3. The method for preparing the N-doped porous carbon composite lithium battery anode material by using the coal humic acid extraction residues as claimed in claim 1 or 2, which is characterized in that:
in the step S2, the mass ratio of the lignite raw material to the urea is 1: 1; the solid-to-liquid ratio (g: mL) of the mixture to the KOH solution is 1: 20; the mass fraction of the KOH solution is 2 percent; then, the prepared solid-liquid mixture is kept for 90min in a water bath with the temperature of 90 ℃;
in step S3: carbonizing and activating for 1h at the temperature of 600 ℃ to obtain a carbonized and activated product;
in step S4: the concentration of the hydrochloric acid solution used was 1.0 mol/L.
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