CN113148973B - Nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, and preparation and application methods thereof - Google Patents

Nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, and preparation and application methods thereof Download PDF

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CN113148973B
CN113148973B CN202110334211.9A CN202110334211A CN113148973B CN 113148973 B CN113148973 B CN 113148973B CN 202110334211 A CN202110334211 A CN 202110334211A CN 113148973 B CN113148973 B CN 113148973B
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porous carbon
phenylenediamine
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CN113148973A (en
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王海鹰
贺颖捷
柴立元
吴弼朝
金林锋
杨志辉
侯兰晶
唐崇俭
刘恢
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Central South University
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    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
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Abstract

The invention provides a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, which is characterized in that the nitrogen content of the nitrogen-doped porous carbon electrode material is 0.86-10.52 at.%, the carbon content is 74.2-93.39 at.%, and the oxygen content is 5.75-15.28 at.%; the particle size of the nitrogen-doped porous carbon electrode material is 0.5-3 mu m, and the specific surface area is 1189-3150 m 2 Per g, pore volume of 0.55-2.30 cm 3 (ii) in terms of/g. The preparation process of the nitrogen-doped porous carbon electrode material comprises the following steps: carrying out polymerization reaction on m-phenylenediamine in aqueous solution containing persulfate, and separating, cleaning and drying a product after the polymerization reaction to obtain poly-m-phenylenediamine particles; mixing the poly (m-phenylenediamine) particles with bicarbonate, and adding N 2 Activating at 600-1000 ℃ in the atmosphere, and cleaning and drying after activation to finally obtain the nitrogen-doped porous carbon electrode material with excellent adsorption performance on hexavalent chromium in water.

Description

Nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, and preparation and application methods thereof
Technical Field
The invention relates to the field of water treatment, in particular to a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, and a preparation method and an application method thereof.
Background
The chromium-containing wastewater is an important pollution source in the industrial processes of metallurgy and the like, the toxicity of hexavalent chromium is high, the human health and the ecological environment are seriously harmed, and the development of the high-efficiency treatment technology of the hexavalent chromium-containing wastewater is urgent. Capacitive Deionization (CDI), chemical precipitation, adsorption, ion exchange, membrane treatment, and the like are the main methods for removing hexavalent chromium. Among them, capacitive deionization has been widely noticed by researchers because of its advantages such as low cost, easy regeneration of electrodes, no secondary pollution, and simple operation.
Currently, the CDI process research at home and abroad mainly focuses on the development of carbon electrode materials, but because of the low specific capacitance of carbon materials, the carbon electrodes have low electric adsorption capacity, and the development and application of CDI are greatly limited. In recent years, nitrogen (N) doping has received much attention from researchers as one of effective means for changing the electronic structure of carbon materials and improving their electrical, chemical, optical, and other properties; however, nitrogen-doped carbon is rarely applied to removing hexavalent chromium by CDI, and the action of nitrogen is not deeply studied, so that the development and application of nitrogen-doped porous carbon in the treatment of hexavalent chromium-containing wastewater are greatly limited, and the result of poor recovery efficiency of hexavalent chromium in the wastewater at present is caused.
In view of the above, it is necessary to provide a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, and a preparation method and an application method thereof, so as to solve or at least alleviate the technical defect of poor recovery efficiency of hexavalent chromium in wastewater.
Disclosure of Invention
The invention mainly aims to provide a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, and preparation and application methods thereof, and aims to solve the technical problem of poor recovery efficiency of hexavalent chromium in wastewater.
In order to achieve the above object, the present invention provides a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, the nitrogen-doped porous carbon electrode material having a nitrogen content of 0.86 to 10.52at.%, a carbon content of 74.2 to 93.39at.%, and an oxygen content of 5.75 to 15.28at.%;
the particle size of the nitrogen-doped porous carbon electrode material is 0.5-3 mu m, and the specific surface area is 1189-3150 m 2 Per g, pore volume of 0.55-2.30 cm 3 /g。
The invention also provides a preparation process of the nitrogen-doped porous carbon electrode material, which comprises the following steps:
s1, performing polymerization reaction on m-phenylenediamine in a persulfate-containing aqueous solution, and then sequentially performing separation operation, first cleaning operation and first drying operation on a product obtained by the polymerization reaction to obtain poly (m-phenylenediamine) particles;
s2, mixing the poly (m-phenylenediamine) particles with bicarbonate, and adding N 2 Activating at 600-1000 deg.C under atmosphere; and sequentially performing a second cleaning operation and a second drying operation on the activated product to obtain the nitrogen-doped porous carbon electrode material.
Further, in the S1, the step of subjecting m-phenylenediamine to polymerization reaction in an aqueous solution containing a persulfate includes: adding the aqueous solution of the persulfate into the aqueous solution of the m-phenylenediamine, and stirring at the temperature of 0-40 ℃ for 0.5-48 h.
Further, in the step S1, the temperature of the stirring treatment is 25 ℃, and the time of the stirring treatment is 8 hours; in the step S2, the activation time is 2h.
Further, in the S1, the molar ratio of the m-phenylenediamine to the persulfate is 1:0.5 to 2;
in the S2, the mass ratio of the poly (m-phenylenediamine) particles to the potassium bicarbonate is 1:3 to 5.
Further, the persulfate includes one of sodium persulfate and ammonium persulfate.
Further, the first washing operation includes: washing a product obtained by the polymerization reaction with an ammonia water solution and an aqueous solution in sequence;
the second cleaning operation comprises: and cleaning the product obtained after activation by using a hydrochloric acid solution and an aqueous solution in sequence.
The invention also provides a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, which is prepared by adopting the preparation process of the nitrogen-doped porous carbon electrode material.
The invention also provides application of the nitrogen-doped porous carbon electrode material in adsorption of hexavalent chromium.
The invention also provides a method for adsorbing hexavalent chromium, which is characterized in that the nitrogen-doped porous carbon electrode material is used on an electrode of a capacitive deionization device;
carrying out hexavalent chromium adsorption treatment on a hexavalent chromium solution with the initial concentration of 50-300mg/L by using the capacitive deionization device; wherein the applied voltage of the capacitive deionization device is 0-1.2V.
Compared with the prior art, the invention has the following advantages:
the nitrogen-doped porous carbon electrode material has excellent electric adsorption performance on hexavalent chromium in a water body, can reach 140.4mg/g, is superior to most of the conventional electrode materials, and is suitable for purifying chromium pollutants in industrial wastewater and underground water; moreover, the nitrogen-doped porous carbon electrode material obtained by the preparation method has a large specific surface area, and in the preparation method, the N content can be regulated and controlled by changing the activation temperature, and the activation temperature can also be set to a specific value, so that the nitrogen-doped porous carbon electrode material with a better adsorption effect on hexavalent chromium in application can be obtained; in addition, the preparation method has simple process and easily controlled conditions, and is easy to realize industrialization.
Drawings
In order to more clearly illustrate the embodiments or technical solutions of the present invention, the drawings used in the embodiments or technical solutions of the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is an SEM image of nitrogen-doped porous carbon electrode materials prepared in examples 1-3;
FIG. 2 is a graph showing the pore size distribution of the nitrogen-doped porous carbon electrode material prepared in examples 1 to 3;
FIG. 3 is the EDS-mapping chart of NPC-800 in example 2;
FIG. 4 is a graph showing the electro-adsorption performance of NPC-600, NPC-800 and NPC-1000 on hexavalent chromium in example 4;
FIG. 5 is a graph showing the effect of NPC-800 in example 5 on the removal of hexavalent chromium at various voltages;
FIG. 6 is a graph showing the effect of NPC-800 on the removal of hexavalent chromium at different concentrations in example 6.
The implementation, functional features and advantages of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive efforts based on the embodiments of the present invention, are within the scope of protection of the present invention.
It should be noted that all the directional indicators (such as upper and lower … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the figure), and if the specific posture is changed, the directional indicator is changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
Moreover, the technical solutions in the embodiments of the present invention may be combined with each other, but it is necessary to be able to be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent, and is not within the protection scope of the present invention.
It will be appreciated by those skilled in the art that the Pore Diameter in the figures can be represented as aperture, q, without affecting the understanding of the present invention e Can be expressed as a saturated Adsorption amount, an Applied voltage can be expressed as an Applied voltage, the removal rate of Cr can be expressed as a chromium removal rate, the initial concentration of Cr can be expressed as an initial concentration of chromium, and an Adsorption amount can be expressed as an Adsorption amount.
In order to improve the recovery efficiency of hexavalent chromium in wastewater, the invention provides a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, which is used in a capacitive deionization device, so that the hexavalent chromium is efficiently adsorbed.
The nitrogen content of the nitrogen-doped porous carbon electrode material can be 0.86-10.52 at.%, the carbon content can be 74.2-93.39 at.%, and the oxygen content can be 5.75-15.28 at.%;
the particle size of the nitrogen-doped porous carbon electrode material can be 0.5-3 mu m, and the specific surface area can be 1189-3150 m 2 The pore volume can be 0.55-2.30 cm 3 (ii) in terms of/g. In the present invention, the size among the above particle sizes may be expressed as a particle diameter.
In addition, in order to further improve the recovery efficiency of hexavalent chromium in wastewater, the nitrogen content of the nitrogen-doped porous carbon electrode material can be 2.21at.%, the carbon content can be 88.15at.%, and the oxygen content can be 9.65at.%;
when the particle size of the nitrogen-doped porous carbon electrode material is 0.5-3 mu m, the specific surface area can be 3150m 2 The pore volume can be 1.52 cm/g 3 /g。
In order to obtain the nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, the invention also provides a preparation process for preparing the nitrogen-doped porous carbon electrode material, which comprises the following steps:
s1, carrying out polymerization reaction on m-phenylenediamine in an aqueous solution containing persulfate, and then sequentially carrying out separation operation, first cleaning operation and first drying operation on a product obtained by the polymerization reaction to obtain poly-m-phenylenediamine particles.
Wherein the separation operation may be performed by suction filtration after the polymerization reaction is completed, so as to obtain the poly-m-phenylenediamine particles. The first washing operation may include: washing a product obtained by the polymerization reaction with an ammonia water solution and an aqueous solution in sequence; the ammonia water may be a diluted solution having a dilution ratio of 50%.
S2, mixing the poly (m-phenylenediamine) particles with bicarbonate, and adding N 2 Activating at 600-1000 deg.C under atmosphere; and sequentially performing a second cleaning operation and a second drying operation on the activated product to obtain the nitrogen-doped porous carbon electrode material.
Wherein the second washing operation may include: washing the product obtained after activation by using a hydrochloric acid solution and an aqueous solution in sequence; the concentration of the hydrochloric acid solution can be generally 0.1-1M, and the dosage can be generally 0.1-2L.
In the embodiment, the nitrogen-doped porous carbon electrode material is synthesized by generating the poly-m-phenylenediamine particles containing nitrogen, utilizing the activation pore-forming effect of potassium bicarbonate and adopting the specific activation treatment process in the step S2; the synthesis process is simple and quick, and the size, specific surface area, N content and pore volume of the product can be adjusted, so that when the product is applied to a capacitance deionization device, the optimal adsorption of hexavalent chromium can be achieved.
The nitrogen-doped porous carbon electrode material prepared by the method has high specific surface area (up to 3150 m) 2 The concentration of the hexavalent chromium is controlled, and the method has the characteristics of/g), controllable N content (0.86-10.52 at.%), hierarchical porosity and the like, greatly improves the electric adsorption performance (140.4 mg/g) on hexavalent chromium, and has a wide industrial prospect.
It is noted that, in the invention, the m-phenylenediamine and the persulfate are used as precursors, and the poly-m-phenylenediamine nanoparticles can be obtained based on the oxidation of the m-phenylenediamine by the persulfate through the ratio adjustment between the m-phenylenediamine and the persulfate; and then activating the poly-m-phenylenediamine by potassium bicarbonate at a specific high temperature, and then cleaning and drying to obtain the nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium.
As a preferable production process of the particles of poly-m-phenylenediamine, in the step S1, the step of subjecting m-phenylenediamine to polymerization reaction in an aqueous solution containing a persulfate includes: adding the aqueous solution of the persulfate into the aqueous solution of the m-phenylenediamine, and stirring at the temperature of 0-40 ℃ for 0.5-48 h; wherein, as a preferable mode, in the step S1, the temperature of the stirring treatment is 25 ℃, and the time of the stirring treatment is 8 hours; the molar ratio of the m-phenylenediamine to the persulfate is 1:0.5 to 2.
With respect to the above embodiment, it is also necessary to know that the persulfate includes one of sodium persulfate and ammonium persulfate.
In addition, in the step S2, the mass ratio of the poly-m-phenylenediamine particles to the potassium hydrogencarbonate is 1:3 to 5; the activation time is 2h, and the specific material proportion and the activation time length during activation are determined, so that various characteristics and characteristics of the product can be better controlled under a specific activation process, and a better effect is achieved.
As a further understanding of the present invention, the present invention also provides a nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium, which is prepared by the preparation process of the nitrogen-doped porous carbon electrode material as described in any of the above embodiments.
In order to embody the application value of the nitrogen-doped porous carbon electrode material, the invention also provides the application of the nitrogen-doped porous carbon electrode material in the adsorption of hexavalent chromium.
In order to realize the application of the nitrogen-doped porous carbon electrode material to the adsorption of hexavalent chromium, the invention also provides a method for adsorbing hexavalent chromium, wherein the nitrogen-doped porous carbon electrode material in any embodiment is used on an electrode of a capacitive deionization device; carrying out hexavalent chromium adsorption treatment on the hexavalent chromium solution with the initial concentration of 50-300mg/L by the capacitance deionization device; wherein the applied voltage of the capacitive deionization device is 0-1.2V.
In addition to the above embodiments, the hexavalent chromium solution may be further defined, for example, the hexavalent chromium solution has an initial pH of 2 and a solution flow rate of 10mL/min.
Specifically, as an alternative, the nitrogen-doped porous carbon material and polyvinylidene fluoride may be mixed, with carbon black in a ratio of 8:1:1 mass ratio, adding N-methyl pyrrolidone, grinding into slurry, and coating on a titanium plate, thereby being used for a capacitive deionization device.
For further illustration of the present invention, the following are listed:
example 1
Nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium and preparation method thereof
1. Weighing 1g (namely 1 mol) of m-phenylenediamine monomer, placing the monomer into a 250mL flat-bottomed flask, adding 100mL deionized water, and magnetically stirring to completely dissolve the m-phenylenediamine to obtain an m-phenylenediamine aqueous solution; 2.6191g (i.e. 1 mol) of sodium persulfate was weighed into a beaker and dissolved in 20mL of deionized water to give an aqueous solution of sodium persulfate.
2. Dropwise adding an aqueous solution of sodium persulfate into a flat-bottomed flask filled with an aqueous solution of m-phenylenediamine, and continuously stirring for 8 hours at 25 ℃ to completely carry out a polymerization reaction; after the polymerization reaction is finished, separating a product obtained by the polymerization reaction through suction filtration, then sequentially cleaning the product with 1:1 ammonia water and deionized water to remove impurities, and drying the product after cleaning to obtain black powder, namely the prepared poly (m-phenylenediamine) particles.
3. 1g of poly (m-phenylenediamine) particles were mixed with 4g of potassium bicarbonate and placed in a corundum boat, N 2 Activating for 2h at 600 ℃ in the atmosphere; and then washing the carbon material by using 0.5M hydrochloric acid solution and aqueous solution, and drying the carbon material at 60 ℃ to obtain black powder, namely the prepared nitrogen-doped porous carbon material for adsorbing hexavalent chromium, which is named as NPC-600.
Wherein the NPC-600 has a nitrogen content of 10.52at.%, a carbon content of 74.2at.%, and an oxygen content of 15.28at.%; the NPC-600 has a particle size of 0.5 to 3 μm and a specific surface area of 1189m 2 Per g, poreVolume of 0.55cm 3 /g。
In addition, those skilled in the art may also refer to FIGS. 1 and 2 in understanding the structure of NPC-600. Wherein, an SEM image of the NPC-600 is shown in FIG. 1, from which the structure of the NPC-600 can be clearly and intuitively understood; the NPC-600 pore size distribution is shown in FIG. 2.
Example 2
Nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium and preparation method thereof
1. Weighing 1g (namely 1 mol) of m-phenylenediamine monomer, placing the monomer into a 250mL flat-bottomed flask, adding 100mL deionized water, and magnetically stirring to completely dissolve the m-phenylenediamine to obtain an m-phenylenediamine aqueous solution; 2.6191g (i.e., 1 mol) of sodium persulfate was weighed into a beaker and dissolved in 20mL of deionized water to provide an aqueous solution of sodium persulfate.
2. Dropwise adding an aqueous solution of sodium persulfate into a flat-bottomed flask filled with an aqueous solution of m-phenylenediamine, and continuously stirring for 8 hours at 25 ℃ to completely carry out a polymerization reaction; after the polymerization reaction is finished, separating a product obtained by the polymerization reaction through suction filtration, then sequentially cleaning the product with 1:1 ammonia water and deionized water to remove impurities, and drying the product after cleaning to obtain black powder, namely the prepared poly (m-phenylenediamine) particles;
3. 1g of poly (m-phenylenediamine) granules were mixed with 4g of potassium bicarbonate and placed in a corundum boat, N 2 Activating for 2h at 800 ℃ in the atmosphere; and then, washing the mixture by using a 0.5M hydrochloric acid solution and an aqueous solution, and drying the mixture at 60 ℃ to obtain black powder, namely the prepared nitrogen-doped porous carbon material for adsorbing hexavalent chromium, which is named as NPC-800.
Wherein the NPC-800 has a nitrogen content of 2.21at.%, a carbon content of 88.15at.%, and an oxygen content of 9.65at.%; the NPC-800 has a particle size of 0.5 to 3 μm and a specific surface area of 3150m 2 G, pore volume of 1.52cm 3 /g。
In addition, those skilled in the art may also refer to FIG. 1, FIG. 2, and FIG. 3 in understanding the structure of the NPC-800. Wherein, an SEM image of the NPC-800 is shown in FIG. 1, from which the structure of the NPC-800 can be clearly and intuitively understood; the NPC-800 pore size distribution is shown in FIG. 2; the EDS-mapping chart (converted from color chart) of NPC-800 is shown in FIG. 3, where it is noted that in FIG. 3, a is SEM chart, b is C element distribution chart, C is O element distribution chart, and d is N element distribution chart.
Example 3
Nitrogen-doped porous carbon electrode material for adsorbing hexavalent chromium and preparation method thereof
1. Weighing 1g (namely 1 mol) of m-phenylenediamine monomer, placing the monomer into a 250mL flat-bottomed flask, adding 100mL deionized water, and magnetically stirring to completely dissolve the m-phenylenediamine to obtain an m-phenylenediamine aqueous solution; 2.6191g (i.e., 1 mol) of sodium persulfate was weighed into a beaker and dissolved in 20mL of deionized water to provide an aqueous solution of sodium persulfate.
2. Dropwise adding the aqueous solution of sodium persulfate into a flat-bottomed flask filled with the aqueous solution of m-phenylenediamine, and continuously stirring for 8 hours at 25 ℃ to completely carry out the polymerization reaction; after the polymerization reaction is finished, separating a product obtained by the polymerization reaction through suction filtration, then sequentially cleaning the product with 1:1 ammonia water and deionized water to remove impurities, and drying the product after cleaning to obtain black powder, namely the prepared poly (m-phenylenediamine) particles.
3. 1g of poly (m-phenylenediamine) granules were mixed with 4g of potassium bicarbonate and placed in a corundum boat, N 2 Activating for 2h at 1000 ℃ in the atmosphere; and then cleaning the mixture by using a 0.5M hydrochloric acid solution and an aqueous solution, and drying the mixture at 60 ℃ to obtain black powder, namely the prepared nitrogen-doped porous carbon material for adsorbing hexavalent chromium, which is named as NPC-1000.
Wherein the NPC-1000 has a nitrogen content of 0.86at.%, a carbon content of 93.39at.%, and an oxygen content of 5.75at.%; the NPC-1000 has a particle size of 0.5 to 3 μm and a specific surface area of 2742m 2 Per g, pore volume of 2.30cm 3 /g。
In addition, those skilled in the art may also refer to FIGS. 1 and 2 in understanding the structure of NPC-1000. Wherein, an SEM image of the NPC-1000 is shown in FIG. 1, from which the structure of the NPC-1000 can be clearly and intuitively understood; the NPC-1000 pore size distribution is shown in FIG. 2.
Example 4
Application of nitrogen-doped porous carbon electrode material in electric adsorption of hexavalent chromium in water body
The NPC-600 prepared in example 1, the NPC-800 prepared in example 2, and the NPC-1000 prepared in example 3 were applied to electrode materials in a capacitive deionization apparatus, respectively, at room temperature, wherein the masses of the NPC-600, NPC-800, and NPC-1000 were all 40mg; the volume of the initial hexavalent chromium solution was 30mL and the initial hexavalent chromium concentration was 200mg/L.
The voltage applied to the capacitive deionization apparatus was set to 1.2V, the adsorption time was set to 10 hours, the flow rate of the solution during adsorption was 10mL/min, and the concentration was measured by spectrophotometry after adsorption.
As shown in FIG. 4, the results of the above experiments indicate that the electro-adsorption capacities of NPC-600, NPC-800 and NPC-1000 reached 125.8mg/g, 140.4mg/g and 96.6mg/g, respectively.
Example 5
And (3) carrying out electric adsorption on hexavalent chromium in the water body by the nitrogen-doped porous carbon electrode material under different voltages.
The NPC-800 prepared in example 2 was applied to an electrode material in a capacitive deionization apparatus at room temperature, the mass of the NPC-800 being 40mg; the volume of the initial hexavalent chromium solution is 30mL, and the concentration of the hexavalent chromium is 200mg/L.
Setting the applied voltage of the capacitance deionization device at 0-1.2V, setting the adsorption time as 10h, setting the solution flow rate in the adsorption process as 10mL/min, and measuring the concentration by adopting a spectrophotometry after adsorption.
As shown in fig. 5, the results of the above experiments indicate that the removal rates of hexavalent chromium reach 60.2%,65.3%,78.1% and 91.8% at 0V, 0.4V, 0.8V and 1.2V, respectively.
Example 6
The N-doped porous carbon electrode material is applied to the electro-adsorption of hexavalent chromium in water bodies with different initial concentrations.
The NPC-800 prepared in example 2 was applied to an electrode material in a capacitive deionization apparatus at room temperature, and the mass of the NPC-800 was 40mg; the volume of the initial hexavalent chromium solution is 30mL, and the concentration of the hexavalent chromium is 20-300 mg/L.
The voltage applied to the capacitive deionization apparatus was set to 1.2V, the adsorption time was set to 10 hours, the flow rate of the solution during adsorption was 10mL/min, and the concentration was measured by spectrophotometry after adsorption.
As shown in FIG. 6, the results of the above experiments revealed that the removal amounts of hexavalent chromium (i.e., the adsorption amounts corresponding to the drawing) were 15.3mg/g, 37.7mg/g, 70.8mg/g, 139.6mg/g and 186.5mg/g, respectively, at initial concentrations of 20mg/L, 50mg/L, 100mg/L, 200mg/L and 300mg/L.
In the above technical solutions, the above are only preferred embodiments of the present invention, and the technical scope of the present invention is not limited thereby, and all the technical concepts of the present invention include the claims of the present invention, which are directly or indirectly applied to other related technical fields by using the equivalent structural changes made in the content of the description and the drawings of the present invention.

Claims (4)

1. The application of the nitrogen-doped porous carbon electrode material in adsorption of hexavalent chromium is characterized in that the nitrogen content of the nitrogen-doped porous carbon electrode material is 0.86-10.52 at.%, the carbon content is 74.2-93.39 at.%, and the oxygen content is 5.75-15.28 at.%;
the particle size of the nitrogen-doped porous carbon electrode material is 0.5-3 mu m, and the specific surface area is 1189-3150 m 2 Per g, pore volume of 0.55-2.30 cm 3 /g;
The preparation process of the nitrogen-doped porous carbon electrode material comprises the following steps:
s1, performing polymerization reaction on m-phenylenediamine in a persulfate-containing aqueous solution, and then sequentially performing separation operation, first cleaning operation and first drying operation on a product obtained by the polymerization reaction to obtain poly (m-phenylenediamine) particles;
the persulfate comprises one of sodium persulfate and ammonium persulfate, and the molar ratio of the m-phenylenediamine to the persulfate is 1:0.5 to 2;
s2, mixing the poly (m-phenylenediamine) particles with bicarbonate, and adding N 2 Activating at 800 deg.C for 2h in the atmosphere; sequentially performing secondary cleaning on the activated productWashing and drying for the second time to obtain the nitrogen-doped porous carbon electrode material;
the bicarbonate is potassium bicarbonate, and the mass ratio of the poly (m-phenylenediamine) particles to the potassium bicarbonate is 1:3 to 5.
2. The use according to claim 1, wherein in said S1, said step of subjecting m-phenylenediamine to polymerization reaction in an aqueous solution containing a persulfate comprises: adding the aqueous solution of the persulfate into the aqueous solution of the m-phenylenediamine, and stirring at the temperature of 0-40 ℃ for 0.5-48 h.
3. The use according to claim 2, wherein in S1, the temperature of the stirring treatment is 25 ℃ and the time of the stirring treatment is 8h.
4. Use according to any one of claims 1 to 3, wherein the first washing operation comprises: washing a product obtained by the polymerization reaction with an ammonia water solution and an aqueous solution in sequence;
the second cleaning operation comprises: and cleaning the product obtained after activation by using a hydrochloric acid solution and an aqueous solution in sequence.
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