CN107369563B - Preparation method of nickel sulfide particle/cellulose-based composite carbon aerogel material - Google Patents
Preparation method of nickel sulfide particle/cellulose-based composite carbon aerogel material Download PDFInfo
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Abstract
The invention discloses a preparation method of a nickel sulfide particle/cellulose-based composite carbon aerogel material. The nickel sulfide/cellulose-based composite carbon aerogel takes one or more of cellulose, nickel salt and sulfur source as raw materials; the preparation process comprises the following steps: dissolving cellulose into a concentrated cellulose solution, and preparing cellulose aerogel through a sol-gel process and a freeze drying technology; preparing cellulose-based carbon aerogel by high-temperature carbonization treatment; nickel sulfide particles were grown in situ on cellulose-based carbon aerogel by one-step solvothermal method. The invention adopts cellulose with wide source and low cost as a precursor, and has no toxic and harmful reagents, and the prepared nickel sulfide particle/cellulose-based composite carbon aerogel has the characteristics of uniform distribution of nickel sulfide particles, high specific surface area, high conductivity and the like, and is an ideal electrode material for new energy devices such as super capacitors, lithium ion batteries and the like.
Description
Technical Field
The invention belongs to the technical field of transition metal sulfide-carbon aerogel, and particularly relates to a nickel sulfide particle/cellulose-based composite carbon aerogel material and a preparation method thereof.
Background
The aerogel is a porous gel substance with a three-dimensional network structure and taking gas as a dispersion medium, the porosity is generally 80-99.8%, and the specific surface area is generally 200-1000 m2g-1The density is usually less than 0.1g cm-3. Since the first aerogel-silica aerogel was produced by Kistler in 1931, polymeric, carbon, and other aerogels were present in succession. In recent years, carbon aerogel has attracted attention and been widely used because of its advantages such as high porosity, low density, high specific surface area, high conductivity, controllable structure and good stability. The carbon aerogel has the advantages of high porosity, high specific surface area and the like, shows strong adsorption capacity and has wide application prospect in the aspects of adsorbents, catalyst carriers and the like; the carbon aerogel has the advantages of high specific surface area, high conductivity, controllable structure, good stability and the like, and can be used as an electrode material of an energy storage device.
Carbon aerogel is used for preparing electrode materials because of high specific surface area, good conductivity and thermal stability, but the specific capacity of the carbon aerogel is low, and formaldehyde, one of common raw materials for preparing the carbon aerogel, is a toxic gas and can generate adverse effects on the environment and human health. Therefore, carbon aerogels are limited in use.
Disclosure of Invention
Aiming at the defects of the carbon aerogel, the invention provides the nickel sulfide particle/cellulose-based composite carbon aerogel which is environment-friendly in preparation process and low in preparation cost, and a preparation method and application thereof.
The invention provides a preparation method of nickel sulfide particles/cellulose-based composite carbon aerogel, which adopts a one-step solvothermal method to grow nickel sulfide particles in situ on a cellulose-based carbon aerogel framework, and comprises the following raw materials: one or more of cellulose, alkali solution, nickel salt and sulfur source, and the method comprises the following steps:
(1) dispersing cellulose in an alkali solution to obtain a semitransparent concentrated cellulose solution;
(2) transferring the concentrated cellulose solution into a mold, and heating in a water bath at the temperature of 50-120 ℃ for 3-6 h to obtain alkaline cellulose hydrogel;
(3) soaking the alkaline cellulose hydrogel in deionized water for 12-72 h to obtain cellulose hydrogel;
(4) freezing the cellulose hydrogel into a solid, and then freeze-drying in a freeze dryer for 12-72 hours to obtain cellulose aerogel;
(5) carbonizing cellulose aerogel at high temperature to obtain cellulose-based carbon aerogel;
(6) dissolving nickel salt and a sulfur source in a proper solvent to prepare a mixed solution containing the nickel source and the sulfur source;
(7) and carrying out solvothermal reaction on the prepared cellulose-based carbon aerogel and a mixed solution containing a nickel source and a sulfur source at 100-220 ℃ for 6-24 h, washing and drying to obtain the nickel sulfide/cellulose-based composite carbon aerogel.
Further, the alkali solution is a mixed solution of sodium hydroxide/urea.
Preferably, the concentrated cellulose solution is prepared by the following steps: firstly dispersing cellulose in a sodium hydroxide/urea mixed solution, then placing the solution in a refrigerator for freezing at the temperature of-18-10 ℃, and then rapidly stirring for a period of time to obtain a concentrated cellulose solution.
Preferably, in the sodium hydroxide/urea mixed solution, the sodium hydroxide accounts for 5-10% of the total weight of the mixed solution, and the urea accounts for 10-15% of the total weight of the mixed solution.
Further, the cellulose comprises plant cellulose, bacterial cellulose and regenerated cellulose, and the cellulose solid content of the concentrated cellulose solution is 1-5%.
Further, in the high-temperature carbonization process in the step (5), the cellulose aerogel is placed in a tube furnace, and the temperature rise program is controlled to be: heating the mixture from room temperature to 500 ℃ for 80-150 min; heating for 20-50 min from 500-800 ℃; and heating the mixture from 800-1000 ℃ for 30-60 min, and preserving the heat for 80-150 min to obtain the cellulose-based carbon aerogel.
Further, the nickel salt in the step (6) is selected from nickel nitrate, nickel sulfate, nickel chloride and nickel acetate, and the concentration of the nickel salt is 5-50 mg mL < -1 >.
Further, the sulfur source in the step (6) is thiourea or sodium sulfide, and the concentration of the sulfur source is 5-20 mg mL < -1 >.
The invention also provides nickel sulfide particles/cellulose-based composite carbon aerogel for growing nickel sulfide particles in situ on a cellulose-based carbon aerogel skeleton by adopting a one-step solvothermal method, which comprises the following raw materials: one or more of cellulose, alkali solution, nickel salt and thiourea.
The invention also provides application of the nickel sulfide particle/cellulose-based composite carbon aerogel as an ideal electrode material of new energy devices such as a super capacitor, a lithium ion battery, a dye-sensitized battery and the like.
The invention has the beneficial effects that:
(1) the method has the advantages of ingenious design idea, adoption of the low-price and environment-friendly cellulose as the main raw material and adoption of the simple, environment-friendly and easy-to-operate preparation process to directly construct the nickel sulfide/cellulose-based composite carbon aerogel.
(2) The nickel sulfide particles on the prepared nickel sulfide particle/cellulose-based composite carbon aerogel skeleton are uniformly distributed and have uniform size, and the high specific capacity of the nickel sulfide is utilized to improve the capacity of the carbon aerogel, so that the electrochemical performance of the composite material is remarkably optimized, and the composite material becomes an ideal electrode material for preparing new energy devices such as high-performance super capacitors, lithium ion batteries, dye-sensitized batteries and the like.
Drawings
FIG. 1a is a scanning electron micrograph of a cellulose-based carbon aerogel prepared in accordance with the present invention;
FIG. 1b is the scanning electron microscope image of the nickel sulfide/cellulose-based composite carbon aerogel prepared in the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
Fully dissolving 20g of sodium hydroxide into 80g of deionized water to prepare a 20 wt% sodium hydroxide solution; 30g of urea is fully dissolved in 70g of deionized water to prepare a 30 wt% urea solution. The sodium hydroxide can also be replaced by other alkaline substances, such as potassium hydroxide and lithium hydroxide.
19g of 20 wt% sodium hydroxide and 19g of 30 wt% urea solution are mixed, 2g of bacterial cellulose is added, and the mixture is transferred into a refrigerator to be frozen, wherein the cooling temperature range is-18-10 ℃. And rapidly stirring the frozen bacterial fiber/sodium hydroxide/urea/water mixed solution to dissolve the cellulose to obtain a concentrated solution of the bacterial cellulose.
And pouring the obtained cellulose concentrated solution into a mould, and heating the mould in water solution for a period of time to obtain the alkaline cellulose hydrogel. Wherein the heating temperature is 50-120 ℃, preferably 60-90 ℃, and the heating time is 1-10 hours, preferably 2-6 hours. And soaking the alkaline cellulose hydrogel in deionized water for 12-72 hours to obtain the cellulose hydrogel.
And (3) rapidly freezing the obtained cellulose hydrogel by using liquid nitrogen, and then freeze-drying for 12-72 hours, preferably 24-28 hours, under the vacuum degree of 10-20 Pa to obtain the cellulose aerogel.
Placing the obtained cellulose aerogel in a tubular furnace, and controlling a heating program under the nitrogen protection atmosphere, namely heating the cellulose aerogel to 500 ℃ at room temperature for 80-150 min; and heating at 500-800 ℃ for 20-50 min, and keeping the temperature for 80-120 min to obtain the cellulose-based carbon aerogel.
600mg of nickel nitrate and 300mg of thiourea were completely dissolved in 30mL of N, N-dimethylformamide by sonication, and 25mg of cellulose-based carbon aerogel was put in the above solution and left for 1 hour. Wherein the nickel nitrate may be replaced by other nickel salts, such as nickel sulfate, nickel chloride, nickel acetate, etc. The thiourea may also be replaced by other sulfur sources such as sodium sulfide, potassium sulfide, and the like. The N, N-dimethylformamide may be replaced by water, N-dimethylacetamide, water/N, N-dimethylformamide, water/N, N-dimethylacetamide and other solvents.
And pouring the mixed solution of the carbon aerogel and the nickel nitrate/thiourea into a 50mL hydrothermal kettle, and placing the hydrothermal kettle in an oven at 100-220 ℃ for heat preservation for 6-24 hours. And after the reaction is finished, washing the obtained nickel sulfide/cellulose-based composite carbon aerogel 3 times by using ethanol and deionized water respectively, and drying in an oven at the temperature of 80-100 ℃ for 6-24 hours to finally obtain the nickel sulfide/cellulose-based composite carbon aerogel.
Example 2
Fully dissolving 10g of sodium hydroxide in 90g of deionized water to prepare a 10 wt% sodium hydroxide solution; fully dissolving 20g of urea in 80g of deionized water to prepare a 20 wt% urea solution. Mixing 99g of 10 wt% sodium hydroxide with 99g of 20 wt% urea solution, adding 2g of plant cellulose, and freezing in a refrigerator at-18-10 ℃. Preparation of nickel sulfide/cellulose-based composite carbon aerogel other procedures were the same as in example 1.
Example 3
Fully dissolving 15g of sodium hydroxide in 85g of deionized water to prepare 15 wt% of sodium hydroxide solution; 25g of urea is fully dissolved in 75g of deionized water to prepare a 25 wt% urea solution. Mixing 49g of 15 wt% sodium hydroxide with 49g of 25 wt% urea solution, adding 2g of bacterial cellulose, and transferring the bacterial cellulose into a refrigerator for freezing, wherein the cooling temperature range is-18-10 ℃. Preparation of nickel sulfide/cellulose-based composite carbon aerogel other procedures were the same as in example 1.
Example 4
The process for preparing the cellulose-based carbon aerogel is the same as in example 1.
The mass of the nickel nitrate and the thiourea was changed to 1500mg and 600mg, respectively, and the nickel sulfide/cellulose-based composite carbon aerogel was prepared as in example 1.
Example 5
The process for preparing the cellulose-based carbon aerogel is the same as in example 1.
The nickel sulfide/cellulose-based composite carbon aerogel can be prepared by changing the mass of the nickel nitrate and the thiourea into 150mg and 150mg respectively as in example 1.
The results of testing the electrochemical properties of the nickel sulfide/cellulose-based composite carbon aerogels obtained in examples 1-5 are shown in table 1. The result shows that the nickel sulfide/cellulose-based composite carbon aerogel obtained by the preparation method provided by the invention has better electrochemical performance and is an ideal electrode material for new energy devices such as super capacitors, lithium ion batteries and the like.
TABLE 1 electrochemical Properties of the nickel sulfide/cellulose-based composite carbon aerogels obtained in examples 1-5
Fig. 1a and 1b are scanning electron micrographs of cellulose-based carbon aerogel and nickel sulfide/cellulose-based composite carbon aerogel prepared in example 1 of the present invention, respectively. The test results of SEM showed: the pore diameter of the inner pores of the cellulose-based carbon aerogel prepared by adopting a sol-gel method, a freeze drying technology and a high-temperature carbonization process is 10-20 microns. The nickel sulfide particles on the nickel sulfide particles/cellulose-based carbon aerogel prepared by the method are uniformly distributed, and the particle size is 2-5 mu m. The SEM test result shows that the nickel sulfide/cellulose-based composite carbon aerogel obtained by the preparation method is an ideal electrode material for new energy devices such as high-performance super capacitors, lithium ion batteries and dye-sensitized batteries more intuitively.
Claims (6)
1. A preparation method of nickel sulfide particles/cellulose-based composite carbon aerogel is characterized in that a one-step solvothermal method is adopted to grow nickel sulfide particles in situ on a cellulose-based carbon aerogel framework, and the preparation raw materials comprise: one or more of cellulose, alkali solution, nickel salt and sulfur source, and the method comprises the following steps:
(1) dispersing cellulose in an aqueous alkali to obtain a semitransparent cellulose concentrated solution, wherein the cellulose concentrated solution is prepared by the following steps of firstly dispersing the cellulose in a sodium hydroxide/urea mixed solution, then placing the solution in a refrigerator for freezing at the temperature of-18-10 ℃, and then rapidly stirring for a period of time to obtain the cellulose concentrated solution, wherein the sodium hydroxide in the sodium hydroxide/urea mixed solution accounts for 5-10% of the total weight of the mixed solution, and the urea accounts for 10-15% of the total weight of the mixed solution;
(2) transferring the concentrated cellulose solution into a mold, and heating in a water bath at the temperature of 50-120 ℃ for 3-6 h to obtain alkaline cellulose hydrogel;
(3) soaking the alkaline cellulose hydrogel in deionized water for 12-72 h to obtain cellulose hydrogel;
(4) freezing the cellulose hydrogel into a solid, and then freeze-drying in a freeze dryer for 12-72 hours to obtain cellulose aerogel;
(5) carrying out high-temperature carbonization on cellulose aerogel, placing the cellulose aerogel in a tubular furnace, and controlling the temperature rise program to be: heating the mixture from room temperature to 500 ℃ for 80-150 min; heating for 20-50 min from 500-800 ℃; heating up to 30-60 min from 800-1000 ℃, and preserving heat for 80-150 min to obtain cellulose-based carbon aerogel;
(6) dissolving nickel salt and a sulfur source in a proper solvent to prepare a mixed solution containing the nickel salt and the sulfur source;
(7) and carrying out solvothermal reaction on the prepared cellulose-based carbon aerogel and a mixed solution containing nickel salt and a sulfur source at 100-220 ℃ for 6-24 h, washing, and drying in an oven at 80-100 ℃ for 6-24 h to obtain the nickel sulfide/cellulose-based composite carbon aerogel.
2. The method for preparing nickel sulfide particle/cellulose-based composite carbon aerogel according to claim 1, wherein the cellulose comprises one or both of plant cellulose and bacterial cellulose, and the cellulose solid content of the concentrated cellulose solution is 1-5%.
3. The method for preparing nickel sulfide particle/cellulose-based composite carbon aerogel according to claim 1, wherein the nickel salt in step (6) is selected from one or more of nickel nitrate, nickel sulfate, nickel chloride and nickel acetate, and the concentration of the nickel salt is 5-50 mg mL-1。
4. The method for preparing nickel sulfide particle/cellulose-based composite carbon aerogel according to claim 1, wherein the sulfur source in step (6) is thiourea or sodium sulfide, and the concentration of the sulfur source is 5-20 mg mL-1。
5. A nickel sulfide particle/cellulose-based composite carbon aerogel obtained by the preparation method according to any one of claims 1 to 4.
6. Use of the nickel sulfide particle/cellulose-based composite carbon aerogel according to claim 5 as an electrode material for a supercapacitor, a lithium ion battery or a dye-sensitized battery.
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| CN108249421A (en) * | 2018-03-13 | 2018-07-06 | 陕西科技大学 | A kind of method that three-dimensional class graphene structural carbon material is prepared using catalyst |
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| CN110380019A (en) * | 2019-06-18 | 2019-10-25 | 华南农业大学 | A kind of metal chalcogenide compound for kalium ion battery/three-dimensional network level hole carbon composite and its preparation method and application |
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