CN112624108A - Preparation method of self-enriched porous carbon aerogel material - Google Patents
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Abstract
The invention relates to a preparation method of a self-enriched porous carbon aerogel material, which comprises the following steps: (1) weighing xanthan gum powder and soybean protein powder, adding the xanthan gum powder and the soybean protein powder into water containing NaCl and NaOH, heating and stirring to obtain a gel solution; (2) and (3) freeze-drying and crushing the obtained gel solution to obtain a carbon precursor, mixing the carbon precursor with an activating agent, calcining at high temperature, and cooling, washing and drying the calcined product to obtain the target product self-enriched porous carbon aerogel material. Compared with the prior art, the self-enriched porous carbon aerogel material prepared by adopting the double-template method has the characteristics of environmental friendliness, safe and environment-friendly preparation process, easiness in operation, high preparation efficiency and low energy consumption, and the prepared porous carbon aerogel material contains abundant mesopores and micropores, is a low-cost biomass-based energy storage material and has wide application prospect and market potential.
Description
Technical Field
The invention belongs to the technical field of carbon material preparation, and relates to a preparation method of a self-enriched porous carbon aerogel material.
Background
Environmental and energy issues due to depletion of fossil fuels are currently of increasing concern. In order to solve these problems, it is important to develop an energy storage device with environmental protection and high efficiency.
Carbon aerogel is widely used as an electrode of EDLCs due to its good electronic conductivity, high specific surface area, good chemical stability, low cost and abundant sources, and xanthan gum is a polysaccharide produced by fermentation of xanthomonas using various organic substances such as glucose, sucrose and various biomass wastes as substrates. Due to the unique structure of the biomacromolecule, the gel is easily formed by self-assembly, so that the carbon aerogel with a three-dimensional structure is further prepared, and due to the excellent electron/ion transmission capacity, the three-dimensional layered porous structure is favorable for improving the energy storage performance. In recent years, the preparation of carbon materials by using biomass as a carbon source gradually becomes a research hotspot, and the utilization of waste biomass xanthan gum to produce advanced materials can also improve the economic benefit of kitchen waste treatment. The results show that high specific surface area carbon aerogel materials are obtained using a strong base as the caustic without posing a serious environmental threat.
However, the carbon aerogel materials produced are uneconomical, environmentally unfriendly, and the like due to the use of large amounts of hazardous chemicals, high operating temperatures, multi-step purification procedures, and the like. Therefore, from the viewpoint of environmental friendliness, a green porous carbon preparation method is in demand.
Disclosure of Invention
The invention aims to provide a preparation method of a self-enriched porous carbon aerogel material, and the prepared biomass-based carbon electrode material forms a layered porous structure and has a wide application prospect.
The self-enrichment porous carbon aerogel material is prepared by adopting a double-template method, the self-enrichment porous carbon aerogel material has the characteristic of environmental friendliness, the preparation process is safe and environment-friendly, the operation is easy, the preparation efficiency is high, the energy consumption is low, and the prepared porous carbon aerogel material contains abundant mesopores and micropores, is a low-cost biomass-based energy storage material, and has wide application prospect and market potential.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a self-enriched porous carbon aerogel material comprises the following steps:
(1) weighing xanthan gum powder and soybean protein powder, adding the xanthan gum powder and the soybean protein powder into water containing NaCl and NaOH, heating and stirring to obtain a gel solution;
(2) and (3) freeze-drying and crushing the obtained gel solution to obtain a carbon precursor, mixing the carbon precursor with an activating agent, calcining at high temperature, and cooling, washing and drying the calcined product to obtain the target product self-enriched porous carbon aerogel material.
Further, in the step (1), the mass ratio of xanthan gum powder, soybean protein powder, NaCl and NaOH is 1: (0.6-1): (0.1-6): (0.1-6).
Further, in the step (1), the heating and stirring temperature is 80-95 ℃ and the time is 1-2 h.
Further, in the step (2), the mass ratio of the carbon precursor to the activator is 1 (1-2).
Further, in the step (2), the activating agent is NaOH.
Further, in the step (2), the temperature of the high-temperature calcination is 500-900 ℃, and the time is 2-6 h.
Further, in the step (2), the washing process specifically comprises: multiple washes with deionized water and brine were used.
Further, in the step (2), drying is performed in a vacuum drying oven.
Further, in the step (2), the drying temperature is 60-110 ℃ and the time is 6-12 h.
Further, in the step (2), the freeze-drying is carried out by using liquid nitrogen.
The nitrogen-doped porous carbon aerogel is prepared by taking waste biomass-based xanthan gum and soybean protein as a carbon source and a nitrogen source. Xanthan-soy protein gel is a self-assembly of two biopolymers in the presence of a template (sodium chloride and a small amount of sodium hydroxide), xanthan being a polysaccharide produced by fermentation of xanthomonas species, using various organic substances as substrates, such as glucose, sucrose and various biomass wastes. In addition, soy protein with high protein content can be used as a model nitrogen source for introducing nitrogen into carbon. Meanwhile, due to the unique structures of the two biopolymers, a gel can be easily formed by their self-assembly, thereby further preparing collagen having a 3D structure. Sodium chloride facilitates the increase of the SSA/graphitization degree and the support of the three-dimensional structure, while sodium hydroxide plays an important role in the formation of micropores. The introduction of the nitrogen dopant provides an additional pseudo capacitor, and the energy storage performance can be improved.
The pyrolysis temperature has great influence on pyrolytic carbon, graphitization degree and nitrogen doping, so that the reaction condition and the doping amount are limited to obtain the maximum specific capacitance, the temperature is too high, the specific surface area of an oxygen-deficient compound which is easily generated is reduced, and the desorption and the embedding of heteroatoms in the material are not facilitated; if the temperature is too low, carbonization is not complete, and if the atmosphere is not controlled well, oxygen-containing functional groups on the surface are too much, impedance is large, conductivity and wettability of the electrode are seriously affected, capacity is naturally poor, and the electrochemical performance of the material is greatly affected.
Compared with the prior art, the invention has the following advantages:
(1) the invention adopts the waste biomass xanthan gum as the raw material, the xanthan gum and the soybean protein are natural renewable resources, the sources are rich, the price is low, the carbon content is high, and the xanthan gum is an environment-friendly material which completely meets the requirement of green chemistry.
(2) The preparation process is simple, and the combination of NaCl and NaOH can not only form a three-dimensional layered porous structure, but also reduce the threat to the environment. The prepared biomass-based carbon electrode material has a three-dimensional network structure, is convenient for subsequent modification and other operations, and has low cost and wide application prospect.
Drawings
FIG. 1 shows self-enriched porous carbon aerogel materials prepared in example 1 at a sweep rate of 10mVs-1CV curve of time.
FIG. 2 shows that the self-enriched porous carbon aerogel material prepared in comparative example 1 was swept at a rate of 10mVs-1CV curve of time.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, unless otherwise specified, raw material reagents and processing techniques are all conventional commercial products or conventional processing techniques in the art.
Example 1:
a self-enriched porous carbon aerogel material and a preparation method thereof specifically comprise the following steps:
1) adding 1g of xanthan gum powder, 0.8g of soy protein powder to 50mL of deionized water containing 5g of NaCl and 0.2g of NaOH;
2) heating the mixed solution to 80 ℃ and continuously stirring for 1h to obtain a gel solution;
3) freeze-drying the obtained gel solution and then crushing to obtain a carbon precursor;
4) mixing the gel freeze-dried powder and an activating agent NaOH according to the mass ratio of 1:1, then carrying out high-temperature calcination at the high-temperature calcination temperature of 500 ℃ for 6h, and cooling to room temperature.
5) And washing the obtained carbon sample with deionized water and hydrochloric acid for multiple times, and placing the carbon sample in a vacuum drying oven for vacuum drying at the temperature of 60 ℃ for 6 hours. Thus obtaining the self-enriched porous carbon aerogel material.
And (3) testing the electrochemical performance of the self-enriched porous carbon aerogel material:
and (3) performing electrochemical performance test on the prepared nitrogen-phosphorus co-doped carbon electrode in a three-electrode system by adopting an electrochemical workstation. The working electrode is a self-enriched porous carbon aerogel material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were tested using 6M KOH solution as the electrolyte.
FIG. 1 shows the sweep rate of the self-enriched porous carbon aerogel material prepared in this example at 10 mV. s-1The CV curve of the material is a symmetrical parallelogram in the figure, which shows that the material has good cyclic stability.
Comparative example 1:
compared with example 1, most of them are the same except that 5g of NaCl and 0.2g of NaOH are changed to only 5g of NaCl as a template when preparing a gel solution;
FIG. 2 shows the sweep rate of the self-enriched porous carbon aerogel material prepared by the comparative example at 10 mV. s-1The CV curve in the process, the CV graph in figure 1 is a symmetrical parallelogram, which shows that sodium chloride and sodium hydroxide are used as templates to play an important role in promoting the formation of micropores and further improving the chemical performance, so that the material has good cycle stability. In fig. 2, the closed curve area in the CV curve of the material is obviously smaller and the surface capacitance is smaller under the condition that only sodium chloride is used as the template, and it can be seen that the performance of the material is more favorably improved by the double-template method of sodium chloride and sodium hydroxide in the embodiment 1.
Example 2:
a preparation method of a self-enrichment porous carbon aerogel material from waste xanthan gum specifically comprises the following steps:
1) adding 1g of xanthan gum powder, 0.8g of soy protein powder to 50mL of deionized water containing 5g of NaCl and 0.2g of NaOH;
2) heating the mixed solution to 80 ℃ and continuously stirring for 1h to obtain a gel solution;
3) freeze-drying the obtained gel solution and then crushing to obtain a carbon precursor;
4) mixing the gel freeze-dried powder and an activating agent NaOH according to the mass ratio of 1:2, then carrying out high-temperature calcination at the temperature of 500 ℃ for 6h, and cooling to room temperature.
5) And washing the obtained carbon sample with deionized water and hydrochloric acid for multiple times, and placing the carbon sample in a vacuum drying oven for vacuum drying at the temperature of 70 ℃ for 6 hours. Thus obtaining the self-enriched porous carbon aerogel material.
And (3) testing the electrochemical performance of the self-enriched porous carbon aerogel material:
and (3) performing electrochemical performance test on the prepared nitrogen-phosphorus co-doped carbon electrode in a three-electrode system by adopting an electrochemical workstation. The working electrode is a self-enriched porous carbon aerogel material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were tested using 6M KOH solution as the electrolyte.
Example 3:
a preparation method of a self-enrichment porous carbon aerogel material from waste xanthan gum specifically comprises the following steps:
1) adding 1g of xanthan gum powder, 0.8g of soy protein powder to 50mL of deionized water containing 5g of NaCl and 0.2g of NaOH;
2) heating the mixed solution to 85 ℃ and continuously stirring for 1h to obtain a gel solution;
3) freeze-drying the obtained gel solution and then crushing to obtain a carbon precursor;
4) mixing the gel freeze-dried powder and an activating agent NaOH according to the mass ratio of 1:1, then carrying out high-temperature calcination at the temperature of 600 ℃ for 6h, and cooling to room temperature.
5) And washing the obtained carbon sample with deionized water and hydrochloric acid for multiple times, and placing the carbon sample in a vacuum drying oven for vacuum drying at the temperature of 80 ℃ for 6 hours. Thus obtaining the self-enriched porous carbon aerogel material.
And (3) testing the electrochemical performance of the self-enriched porous carbon aerogel material:
and (3) performing electrochemical performance test on the prepared nitrogen-phosphorus co-doped carbon electrode in a three-electrode system by adopting an electrochemical workstation. The working electrode is a self-enriched porous carbon aerogel material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were tested using 6M KOH solution as the electrolyte.
Example 4:
a preparation method of a self-enrichment porous carbon aerogel material from waste xanthan gum specifically comprises the following steps:
1) adding 1g of xanthan gum powder, 0.8g of soy protein powder to 50mL of deionized water containing 5g of NaCl and 0.2g of NaOH;
2) heating the mixed solution to 90 ℃ and continuously stirring for 2h to obtain a gel solution;
3) freeze-drying the obtained gel solution and then crushing to obtain a carbon precursor;
4) mixing the gel freeze-dried powder and an activating agent NaOH according to a mass ratio of 1:2, then carrying out high-temperature calcination at 700 ℃ for 3h, and cooling to room temperature.
5) And washing the obtained carbon sample with deionized water and hydrochloric acid for multiple times, and placing the carbon sample in a vacuum drying oven for vacuum drying at the temperature of 90 ℃ for 7 hours. Thus obtaining the self-enriched porous carbon aerogel material.
And (3) testing the electrochemical performance of the self-enriched porous carbon aerogel material:
and (3) performing electrochemical performance test on the prepared nitrogen-phosphorus co-doped carbon electrode in a three-electrode system by adopting an electrochemical workstation. The working electrode is a self-enriched porous carbon aerogel material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were tested using 6M KOH solution as the electrolyte.
Example 5:
a preparation method of a self-enriched porous carbon aerogel material from waste xanthan gum comprises the following steps:
1) adding 1g of xanthan gum powder, 0.8g of soy protein powder to 50mL of deionized water containing 5g of NaCl and 0.2g of NaOH;
2) heating the mixed solution to 95 ℃ and continuously stirring for 2h to obtain a gel solution;
3) freeze-drying the obtained gel solution and then crushing to obtain a carbon precursor;
4) mixing the gel freeze-dried powder and an activating agent NaOH according to the mass ratio of 1:1, then carrying out high-temperature calcination at the temperature of 800 ℃ for 3h, and cooling to room temperature.
5) The obtained carbon sample is washed by deionized water and hydrochloric acid for a plurality of times and is placed in a vacuum drying oven for vacuum drying at the temperature of 100 ℃ for 12 hours. Thus obtaining the self-enriched porous carbon aerogel material.
And (3) testing the electrochemical performance of the self-enriched porous carbon aerogel material:
and (3) performing electrochemical performance test on the prepared nitrogen-phosphorus co-doped carbon electrode in a three-electrode system by adopting an electrochemical workstation. The working electrode is a self-enriched porous carbon aerogel material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were tested using 6M KOH solution as the electrolyte.
Example 6:
a preparation method of a self-enriched porous carbon aerogel material from waste xanthan gum comprises the following steps:
1) adding 1g of xanthan gum powder, 0.8g of soy protein powder to 50mL of deionized water containing 5g of NaCl and 0.2g of NaOH;
2) heating the mixed solution to 90 ℃ and continuously stirring for 2h to obtain a gel solution;
3) freeze-drying the obtained gel solution and then crushing to obtain a carbon precursor;
4) mixing the gel freeze-dried powder and an activating agent NaOH according to a mass ratio of 1:2, then carrying out high-temperature calcination at 900 ℃ for 3h, and cooling to room temperature.
5) And washing the obtained carbon sample with deionized water and hydrochloric acid for multiple times, and placing the carbon sample in a vacuum drying oven for vacuum drying to obtain the self-enrichment porous carbon aerogel material.
And (3) testing the electrochemical performance of the self-enriched porous carbon aerogel material:
and (3) performing electrochemical performance test on the prepared nitrogen-phosphorus co-doped carbon electrode in a three-electrode system by adopting an electrochemical workstation. The working electrode is a self-enriched porous carbon aerogel material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were tested using 6M KOH solution as the electrolyte.
Example 7:
a preparation method of a self-enriched porous carbon aerogel material from waste xanthan gum comprises the following steps:
1) adding 1g of xanthan gum powder, 0.8g of soy protein powder to 50mL of deionized water containing 5g of NaCl and 0.2g of NaOH;
2) heating the mixed solution to 95 ℃ and continuously stirring for 2h to obtain a gel solution;
3) freeze-drying the obtained gel solution and then crushing to obtain a carbon precursor;
4) mixing the gel freeze-dried powder and an activating agent NaOH according to the mass ratio of 1:1, then carrying out high-temperature calcination at the temperature of 500 ℃ for 3h, and cooling to room temperature.
5) And washing the obtained carbon sample with deionized water and hydrochloric acid for multiple times, and placing the carbon sample in a vacuum drying oven for vacuum drying at the temperature of 110 ℃ for 12 hours. Thus obtaining the self-enriched porous carbon aerogel material.
And (3) testing the electrochemical performance of the self-enriched porous carbon aerogel material:
and (3) performing electrochemical performance test on the prepared nitrogen-phosphorus co-doped carbon electrode in a three-electrode system by adopting an electrochemical workstation. The working electrode is a self-enriched porous carbon aerogel material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were tested using 6M KOH solution as the electrolyte.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The preparation method of the self-enriched porous carbon aerogel material is characterized by comprising the following steps:
(1) weighing xanthan gum powder and soybean protein powder, adding the xanthan gum powder and the soybean protein powder into water containing NaCl and NaOH, heating and stirring to obtain a gel solution;
(2) and (3) freeze-drying and crushing the obtained gel solution to obtain a carbon precursor, mixing the carbon precursor with an activating agent, calcining at high temperature, and cooling, washing and drying the calcined product to obtain the target product self-enriched porous carbon aerogel material.
2. The preparation method of the self-enriched porous carbon aerogel material according to claim 1, wherein in the step (1), the mass ratio of xanthan gum powder, soybean protein powder, NaCl and NaOH is 1: (0.6-1): (0.1-6): (0.1-6).
3. The preparation method of the self-enriched porous carbon aerogel material according to claim 1, wherein in the step (1), the heating and stirring temperature is 80-95 ℃ and the time is 1-2 h.
4. The preparation method of the self-enriched porous carbon aerogel material according to claim 1, wherein in the step (2), the mass ratio of the carbon precursor to the activator is 1 (1-2).
5. The method for preparing the self-enriched porous carbon aerogel material according to claim 1, wherein in the step (2), the activating agent is NaOH.
6. The method for preparing a self-enriched porous carbon aerogel material as claimed in claim 1, wherein the high-temperature calcination in step (2) is performed at 500-900 ℃ for 2-6 h.
7. The method for preparing the self-enriched porous carbon aerogel material according to claim 1, wherein in the step (2), the washing process specifically comprises the following steps: multiple washes with deionized water and brine were used.
8. The preparation method of the self-enriched porous carbon aerogel material according to claim 1, wherein in the step (2), the drying is performed in a vacuum drying oven.
9. The preparation method of the self-enriched porous carbon aerogel material according to claim 1 or 8, wherein in the step (2), the drying temperature is 60-110 ℃ and the drying time is 6-12 h.
10. The method for preparing the self-enriched porous carbon aerogel material according to claim 1, wherein in the step (2), the freeze-drying is performed by using liquid nitrogen.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114890417A (en) * | 2022-02-21 | 2022-08-12 | 江苏联兴成套设备制造有限公司 | Method for preparing activated carbon aerogel by sodium salt coupling organic matter catalytic activation |
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| US5567812A (en) * | 1994-04-15 | 1996-10-22 | The United States Of America, As Represented By The Secretary Of Agriculture | Polysaccharide products derived from lesquerella fendleri and methods of their production |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114890417A (en) * | 2022-02-21 | 2022-08-12 | 江苏联兴成套设备制造有限公司 | Method for preparing activated carbon aerogel by sodium salt coupling organic matter catalytic activation |
| CN114890417B (en) * | 2022-02-21 | 2023-08-22 | 江苏联兴成套设备制造有限公司 | Method for preparing activated carbon aerogel by catalytic activation of sodium salt coupled organic matter |
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