CN110627065B - Preparation method and application of jute-based nitrogen-containing porous carbon - Google Patents
Preparation method and application of jute-based nitrogen-containing porous carbon Download PDFInfo
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Abstract
The invention belongs to the field of inorganic nano materials, and relates to a nitrogen-containing porous carbon material with a high specific area prepared by utilizing jute fabric, in particular to a preparation method and application of jute-based nitrogen-containing porous carbon. Washing jute fabric, soaking, loading activating agent potassium oxalate and nitrogen-containing precursor urea, putting the jute fabric into a tubular furnace, and carbonizing the jute fabric at high temperature in an inert protective atmosphere to obtain the nitrogen-containing porous carbon. Experimental results show that the material has high specific surface area, good hydrophilicity and stability, the adsorption capacity for low-concentration anionic dye methyl orange can reach 755.18mg/g, and the performance is superior to that of commercial activated carbon powder and most of reported biomass-based nitrogen-containing porous carbons. The preparation method is simple and convenient, the raw materials are renewable resources, the cost is low, the production efficiency is high, and the large-scale industrial application is easy.
Description
Technical Field
The invention belongs to the field of inorganic nano materials, and relates to a nitrogen-containing porous carbon material with a high specific area prepared by utilizing jute fabric, in particular to a preparation method and application of jute-based nitrogen-containing porous carbon.
Background
The porous carbon material has the advantages of high specific surface area, clear pore structure, good thermal stability and chemical stability, high conductivity, low density and the like, and is widely applied to the aspects of pollutant adsorption, energy storage energy conversion, electrochemical sensing and the like. Conventional porous carbon materials (e.g., activated carbon) are typically prepared by pyrolysis or hydrothermal treatment, followed by activation of the organic precursor via chemical or physical methods, which is relatively costly. In addition, pure carbon materials have the disadvantages of strong hydrophobicity, poor electron donating ability, and the like, which limits the application range of the pure carbon materials, and therefore, carbon materials are usually modified by doping other heteroatoms. The nitrogen atom is very close in structure to the carbon atom, and the carbon atom can be replaced by the nitrogen atom by controlling the preparation process. The nitrogen atoms are introduced into the porous carbon material, so that the pore structure of the porous carbon material can be adjusted, the surface composition of the material is changed, the hydrophilicity of the material is improved, the conductivity of the material is enhanced, and the application range of the porous carbon material is greatly expanded.
The preparation of nitrogen-containing porous carbon materials based on renewable biomass resources and their application in the fields of adsorption, batteries, supercapacitors and the like have attracted extensive attention of researchers. The biomass-derived porous carbon is not only environment-friendly and low in cost, but also easy to prepare. Biomass refers to a plant, plant-derived, animal-derived, industrial, sewage-derived, or municipal waste-derived material that can be used to synthesize porous carbon materials and perform a variety of applications. Currently, the most common precursors for synthesizing various porous carbon materials are cherry stone, coffee shell, banana peel, almond shell, corn cob, cotton stalk, date core, olive core, rice bran, rice hull, straw, bagasse, sawdust, tea waste, walnut shell, durian shell, herb residue, apricot residue, orange peel, oil palm fiber, coconut shell, etc. (see (Auto M, Hamed B H. Preparation of waste Activated carbon using porous acetic Acid as an activating agent for addition of Acid Blue 25. J. Chemical Engineering Journal, 2011, 171(2): 502. 509.), (Gonz lez-Dom I. J. M, Alexander-Franco M, Fern. Fe-z-actuating J. C. ceramic, calcium carbonate J. activating agent, calcium carbonate J. copper, calcium carbonate, 2017, 37(2): 148-; (Wong S, Ngadi N, Inuwa I M, et al. Recent advances in applications of activated carbon from biological for water treatment. a short review [ J ] Journal of Cleaner Production, 2018, 175: 361-.
Porous carbon prepared by directly pyrolyzing a biomass precursor has limited pore structure, is mainly porous carbon with a microporous structure, and is difficult to obtain a hierarchical pore structure. The hierarchical pore structure with a certain micropore-mesopore-macropore structure can be obtained by rapid heating (50 ℃/s). But their specific surface area and pore structure are still weak, and physical or chemical activation methods are commonly used to develop their pore structure. Physical activation typically employs an oxidizing gas (e.g., O)2、CO2Or water vapor) (see (Siyasukh A, Chimupa Y, Tonan N. Preparation of magnetic resonance carbon spheres with graphical defects for high-methyl oxygen adsorption capacity [ J]Carbon, 2018, 134: 207-. Generally speaking, chemical activation has advantages over physical activation, such as relatively low activation temperature, short activation time, fringing porous carbon pore structure, and high specific surface area and pore volume. The disadvantage is that the activator has to be washed off after activation. The properties of the porous carbon are greatly influenced by the activator, and the type of the activator, the proportion of the activator and the activation conditions influence the pore structure of the porous carbon. Commonly used activators are mainly ZnCl2、KOH/NaOH、KHCO3、H3PO4Etc. (see; (Nitto-Delgado C, Partida-Guitrez D, Range-Mendez J R. Preparation of activated carbon rings from recycled fabrics and their performance reducing the adaptation of model and organic polutants in water [ J ] J]. Journal of cleaner production, 2019, 213: 650-658.）；（Khan J H, Marpaung F, Young C, et al. Jute-derived microporous/mesoporous carbon with ultra-high surface area using a chemical activation pr℃ess[J]Microporous and Mesoporous Materials, 2019, 274: 251-. Wherein, ZnCl2The mesoporous is mainly developed, and the activity is mild; KOH/NaOH has low activation temperature and is widely used, but the sample has stronger corrosivity, and the yield of the obtained porous carbon is lower. KHCO3The gas can be generated by thermal decomposition, which is more beneficial to obtaining the porous carbon with the hierarchical structure. H3PO4The method is widely used for activating lignocellulose biomass, mainly develops micropores and mesopores, but has a limited applicable biomass range. Therefore, the exploration and development of the activating agent with high activity, high yield, low toxicity and low cost still have important significance for preparing the biomass nitrogen-containing porous carbon material.
In addition, screening of new biomass raw materials with low price and wide sources is also an effective method for expanding biomass porous carbon materials and realizing resource recycling of biomass. The jute fiber has the characteristics of high yield, wide source, low price, high fiber strength and the like, and is very suitable for preparing nitrogen-containing porous carbon.
Disclosure of Invention
The invention provides a preparation method and application of jute-based nitrogen-containing porous carbon, which solve the technical problem of preparing nitrogen-containing porous carbon with high specific area and high anionic dye adsorption capacity by using jute fabric.
The technical scheme of the invention is realized as follows:
a preparation method of nitrogen-containing porous carbon based on jute comprises the following steps:
(1) pretreatment of jute: soaking and washing jute cloth strips by deionized water and ethanol, and drying in an oven;
(2) loading of activator and nitrogen-containing precursor: dipping the jute cloth strips treated in the step (1) in a solution containing an activating agent and a nitrogen-containing precursor, taking out and placing in an oven for drying to obtain loaded jute cloth strips;
(3) high-temperature carbonization: placing the loaded jute cloth strips in a tubular furnace, heating and carbonizing under protective gas, and naturally cooling to room temperature to obtain a carbonized sample;
(4) washing and drying: and soaking the carbonized sample in dilute hydrochloric acid, fully washing the carbonized sample with deionized water, and finally drying the carbonized sample in an oven to obtain the nitrogen-containing porous carbon.
In the step (2), the activating agent is potassium oxalate and the nitrogen-containing precursor is urea; the mass concentration of potassium oxalate is 0.1-2.5 mol/L; the dipping time is 0.5-15 h.
The mass ratio of the jute cloth strips to the activating agent to the nitrogen-containing precursor is 1: (1.38-34.47): (0 to 0.4).
The carbonization temperature in the step (3) is 500-.
The protective gas is one or more of nitrogen, argon or helium, and the flow rate is 5-50 mL/min.
The concentration of the dilute hydrochloric acid in the step (4) is 0.1-2 mol/L.
The drying temperature in the oven is 60-100 ℃, and the drying time is 6-12 h.
The prepared nitrogen-containing porous carbon is applied to the aspect of adsorbing a large amount of methyl orange.
The specific surface area of the nitrogen-containing porous carbon is 800-1500 m2The pore diameter of the material is 0.6-1.9nm, and the nitrogen content is 0.5-10 wt%.
The invention has the following beneficial effects:
the invention selects potassium oxalate which can generate effective corrosive and more gas-phase escaping substances through pyrolysis as an activating agent, and is beneficial to the prepared nitrogenous porous carbon to obtain higher specific surface area and porosity. The experimental result shows that the maximum specific surface area of the material is as high as 1188.6 m2The adsorption capacity of the low-concentration anionic dye methyl orange can reach 755.18mg/g, and the performance of the low-concentration anionic dye methyl orange is superior to that of commercial activated carbon powder and most of reported biomass-based nitrogen-containing porous carbon;
secondly, the activating agent and the nitrogen-containing precursor can be loaded on the inner surface and the outer surface of the jute fabric by adopting an impregnation method, so that the uniform dispersion of the activating agent and the nitrogen-containing precursor is favorably realized, and the effectiveness and uniformity of pore-forming and nitrogen doping are improved;
thirdly, renewable jute fabric is selected as a base material, and on one hand, the fabric structure can be reserved after carbonization of the jute fabric to prepare a cloth-like nitrogen-containing porous carbon material, so that the collection operation of a sample and better dispersion, separation and recovery during actual adsorption use are facilitated; on the other hand, the recovery and high value-added utilization of a large amount of jute waste fabrics can be realized. The synthesis method is simple and convenient, the sources of the required raw materials are rich, the price is low, and the industrial production and application are easy to realize.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a scanning electron microscope image of the nitrogen-containing porous carbon prepared by the nitrogen-containing porous carbon preparation method of the present invention.
FIG. 2 is a graph showing the isothermal adsorption curve and the pore size distribution of the nitrogen-containing porous carbon prepared by the method for preparing the nitrogen-containing porous carbon of the present invention.
FIG. 3 is a graph showing the adsorption profile of methyl orange by the nitrogen-containing porous carbon prepared by the method.
FIG. 4 is a graph comparing adsorption curves of nitrogen-containing porous carbon material, commercial activated carbon powder and activated carbon particles of example 1 to a methyl orange solution.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The method for preparing nitrogen-containing porous carbon based on jute is specifically performed according to the following steps:
(1) cutting and cleaning a sample: taking a jute cloth strip (the gram weight is 669.4 g/m) with the length and width of (5 cm multiplied by 2 cm)2) Soaking and ultrasonically washing a plurality of blocks by using deionized water and ethanol (the ultrasonic power is 150W, and the ultrasonic frequency is 60 kHz) for 10min, and then drying the blocks in a blast drying oven at 80 ℃ for 12 h;
(2) loading an activating agent and a nitrogen-containing precursor: preparing 50mL of 1.5mol/L solution from 13.8170g of potassium oxalate crystals, and adding 0.1336g of urea into the solution; then, soaking 0.6681g of 2 pieces of dried jute cloth strips in the solution, taking the jute cloth strips out after 12h, and drying in an oven at 80 ℃ for 12 h;
(3) high-temperature carbonization: putting the loaded jute cloth strips into a corundum crucible, then putting the corundum crucible into a tubular furnace, vacuumizing the air in the tubular furnace for 10min by using a circulating water type vacuum pump, then introducing nitrogen as protective gas, wherein the flow rate is 25mL/min, setting the program to carry out high-temperature carbonization, the initial temperature is 25 ℃, the carbonization setting temperature is 700 ℃, the temperature is increased by 5 ℃ per minute, keeping the temperature for 2h when the temperature is increased to 700 ℃, then reducing the temperature to the room temperature at the speed of 3.7 ℃/min, and taking out a sample after the temperature is 80 ℃ to obtain the nitrogen-containing porous carbon material;
(4) washing and drying: the obtained carbonized sample is soaked and washed for 3 times by 30mL of dilute hydrochloric acid with the concentration of 1mol/L, and is soaked and washed by deionized water until the pH value is close to 7. Finally, the mixture is dried in an oven at 80 ℃ for 12h for standby.
Fig. 1 is an SEM photograph of the nitrogen-containing porous carbon material prepared according to this example. As can be seen from FIG. 1a, the sample obtained after carbonization still maintains the bundle-like structure of jute fiber; as can be seen from FIG. 1b, many micro pores appear on the cross section of the nitrogen-containing porous carbon fiber obtained by potassium oxalate activation, and the pore diameter distribution is mostly below 150 nm. In addition, the nitrogen content of the nitrogen-containing porous carbon sample is tested to be 3.95 wt%.
Example 2
The method for preparing nitrogen-containing porous carbon based on jute is specifically performed according to the following steps:
(1) cutting and cleaning a sample: getJute cloth strip (gram weight 669.4 g/m) with length and width dimensions of (5 cm × 2 cm)2) Soaking and ultrasonically washing a plurality of blocks by using deionized water and ethanol (the ultrasonic power is 100W, the ultrasonic frequency is 40 kHz) for 10min, and then drying the blocks in a 60 ℃ blast drying oven for 6 h;
(2) loading an activating agent and a nitrogen-containing precursor: 23.0288g of potassium oxalate crystals are taken to prepare 50mL of solution with the concentration of 2.5mol/L without adding urea; then, soaking 0.6681g of 2 pieces of dried jute cloth strips in the solution, taking the jute cloth strips out after 12h, and drying in an oven at 80 ℃ for 12 h;
(3) high-temperature carbonization: putting the loaded jute cloth strips into a corundum crucible, then putting the corundum crucible into a tubular furnace, vacuumizing the air in the tubular furnace for 10min by using a circulating water type vacuum pump, then introducing nitrogen as protective gas, wherein the flow rate is 25mL/min, setting the program to carry out high-temperature carbonization, the initial temperature is 25 ℃, the carbonization setting temperature is 700 ℃, the temperature is increased by 5 ℃ per minute, keeping the temperature for 2h when the temperature is increased to 700 ℃, then reducing the temperature to the room temperature at the speed of 3.7 ℃/min, and taking out a sample after the temperature is 80 ℃ to obtain the nitrogen-containing porous carbon material;
(4) washing and drying: the obtained carbonized sample is soaked and washed for 3 times by 30mL of dilute hydrochloric acid with the concentration of 1mol/L, and is soaked by deionized water and then washed until the pH value is close to 7, and finally, the carbonized sample is dried in an oven at 80 ℃ for 12 hours for later use.
The specific surface area is tested to be 1188.6 m2The pore diameter is mainly distributed between 0.59nm and 1.86nm, a small amount of the sample has the pore diameter between 46.32nm and 50.60nm, the nitrogen content is 0.78 weight percent, and the maximum adsorption capacity of the sample on methyl orange at normal temperature is 452.21 mg/g.
Example 3
The method for preparing nitrogen-containing porous carbon based on jute is specifically performed according to the following steps:
(1) cutting and cleaning a sample: taking a jute cloth strip (the gram weight is 669.4 g/m) with the length and width of (5 cm multiplied by 2 cm)2) Soaking several blocks in deionized water and ethanol respectively, ultrasonically washing (ultrasonic power of 150W and ultrasonic frequency of 60 kHz) for 10min, and drying in 80 deg.C blast drying ovenDrying for 12 h;
(2) loading an activating agent and a nitrogen-containing precursor: preparing 18.4230g of potassium oxalate crystals into 50mL of solution with the concentration of 2.0mol/L, and adding 0.1336g of urea into the solution; then, soaking 0.6681g of 2 pieces of dried jute cloth strips in the solution, taking the jute cloth strips out after 12h, and drying in an oven at 80 ℃ for 12 h;
(3) high-temperature carbonization: putting the loaded jute cloth strips into a corundum crucible, then putting the corundum crucible into a tubular furnace, vacuumizing the air in the tubular furnace for 10min by using a circulating water type vacuum pump, then introducing nitrogen as protective gas, wherein the flow rate is 25mL/min, setting the program to carry out high-temperature carbonization, the initial temperature is 25 ℃, the carbonization setting temperature is 700 ℃, the temperature is increased by 5 ℃ per minute, keeping the temperature for 2h when the temperature is increased to 700 ℃, then reducing the temperature to the room temperature at the speed of 3.7 ℃/min, and taking out a sample after the temperature is 80 ℃ to obtain the nitrogen-containing porous carbon material;
(4) washing and drying: and soaking and washing the obtained carbonized sample for 3 times by using 30mL of dilute hydrochloric acid with the concentration of 1mol/L, soaking and washing the carbonized sample by using deionized water until the pH value is close to 7, and finally drying the carbonized sample in an oven at the temperature of 80 ℃ for 12 hours to obtain the nitrogenous porous carbon material.
Example 4
The method for preparing nitrogen-containing porous carbon based on jute is specifically performed according to the following steps:
(1) cutting and cleaning a sample: taking a jute cloth strip (the gram weight is 669.4 g/m) with the length and width of (5 cm multiplied by 2 cm)2) Soaking and ultrasonically washing a plurality of blocks by using deionized water and ethanol (the ultrasonic power is 150W, and the ultrasonic frequency is 60 kHz) for 10min, and then drying the blocks in a blast drying oven at 80 ℃ for 12 h;
(2) loading an activating agent and a nitrogen-containing precursor: preparing 23.0288g of potassium oxalate crystals into 50mL of solution with the concentration of 2.5mol/L, and adding 0.2672g of urea into the solution; then, soaking 0.6681g of 2 pieces of dried jute cloth strips in the solution, taking the jute cloth strips out after 12h, and drying in an oven at 80 ℃ for 12 h;
(3) high-temperature carbonization: putting the loaded jute cloth strips into a corundum crucible, then putting the corundum crucible into a tubular furnace, vacuumizing the air in the tubular furnace for 10min by using a circulating water type vacuum pump, then introducing nitrogen as protective gas, wherein the flow rate is 25mL/min, setting the program to carry out high-temperature carbonization, the initial temperature is 25 ℃, the carbonization setting temperature is 700 ℃, the temperature is increased by 5 ℃ per minute, keeping the temperature for 2h when the temperature is increased to 700 ℃, then reducing the temperature to the room temperature at the speed of 3.7 ℃/min, and taking out a sample after the temperature is 80 ℃ to obtain the nitrogen-containing porous carbon material;
(4) washing and drying: and soaking and washing the obtained carbonized sample for 3 times by using 30mL of dilute hydrochloric acid with the concentration of 1mol/L, soaking and washing the carbonized sample by using deionized water until the pH value is close to 7, and finally drying the carbonized sample in an oven at the temperature of 80 ℃ for 12 hours to obtain the nitrogenous porous carbon material.
Example 5
The method for preparing nitrogen-containing porous carbon based on jute is specifically performed according to the following steps:
(1) cutting and cleaning a sample: taking a jute cloth strip (the gram weight is 669.4 g/m) with the length and width of (5 cm multiplied by 2 cm)2) Soaking and ultrasonically washing a plurality of blocks by using deionized water and ethanol (the ultrasonic power is 150W, and the ultrasonic frequency is 60 kHz) for 10min, and then drying the blocks in a blast drying oven at 80 ℃ for 12 h;
(2) loading an activating agent and a nitrogen-containing precursor: preparing 50mL of solution with the concentration of 0.1mol/L by using 0.9212g of potassium oxalate crystals, and adding 0.2672g of urea into the solution; then, soaking 0.6681g of 2 pieces of dried jute cloth strips in the solution, taking the jute cloth strips out after 2h, and drying in an oven at 100 ℃ for 6 h;
(3) high-temperature carbonization: putting the loaded jute cloth strips into a corundum crucible, then putting the corundum crucible into a tubular furnace, vacuumizing the air in the tubular furnace for 10min by using a circulating water type vacuum pump, then introducing nitrogen as protective gas, wherein the flow rate is 15mL/min, setting the program to carry out high-temperature carbonization, the initial temperature is 25 ℃, the carbonization setting temperature is 500 ℃, the temperature is increased by 3 ℃ per minute, carrying out heat preservation carbonization for 1h when the temperature is increased to 500 ℃, then reducing the temperature to the room temperature at the speed of 3.7 ℃/min, and taking out a sample after the temperature is 80 ℃ to obtain the nitrogen-containing porous carbon material;
(4) washing and drying: and soaking and washing the obtained carbonized sample for 3 times by using 30mL of dilute hydrochloric acid with the concentration of 0.1mol/L, soaking and washing the carbonized sample by using deionized water until the pH value is close to 7, and finally drying the carbonized sample in an oven at 80 ℃ for 12 hours to obtain the nitrogenous porous carbon material.
Example 6
The method for preparing nitrogen-containing porous carbon based on jute is specifically performed according to the following steps:
(1) cutting and cleaning a sample: taking a jute cloth strip (the gram weight is 669.4 g/m) with the length and width of (5 cm multiplied by 2 cm)2) The number of blocks is 1.5g in total, and the blocks are respectively soaked in deionized water and ethanol and ultrasonically washed for 10min (the ultrasonic power is 200W, and the ultrasonic frequency is 100 kHz), and then are placed in a blast drying oven at the temperature of 80 ℃ for drying for 12 h;
(2) loading an activating agent and a nitrogen-containing precursor: preparing 0.9212g of potassium oxalate crystals into 50mL of solution with the concentration of 0.1mol/L, and adding 0.0067g of urea into the solution; then, soaking 0.6681g of 2 pieces of dried jute cloth strips in the solution, taking the jute cloth strips out after 2h, and drying in an oven at 100 ℃ for 6 h;
(3) high-temperature carbonization: putting the loaded jute cloth strips into a corundum crucible, then putting the corundum crucible into a tubular furnace, vacuumizing the air in the tubular furnace for 10min by using a circulating water type vacuum pump, then introducing nitrogen as protective gas, wherein the flow rate is 15mL/min, setting the program to carry out high-temperature carbonization, the initial temperature is 25 ℃, the carbonization setting temperature is 1000 ℃, the temperature is increased by 8 ℃ per minute, carrying out heat preservation carbonization for 3h when the temperature is increased to 1000 ℃, then reducing the temperature to room temperature at the speed of 3.7 ℃/min, and taking out a sample after the temperature is 80 ℃ to obtain a nitrogen-containing porous carbon material;
(4) washing and drying: and soaking and washing the obtained carbonized sample for 3 times by using 30mL of dilute hydrochloric acid with the concentration of 0.1mol/L, soaking and washing the carbonized sample by using deionized water until the pH value is close to 7, and finally drying the carbonized sample in an oven at 80 ℃ for 12 hours to obtain the nitrogenous porous carbon material.
Examples of the effects of the invention
N at 77K for nitrogen-containing porous carbon material prepared in example 12The adsorption and desorption curves and the pore size distribution diagram are shown in FIG. 2. According to the fact that the adsorption and desorption curve belongs to a typical I-type isotherm, the sample is indicated to be mainly of a microporous structure. By passingThe specific surface area of the sample was calculated to be 1368.6m by using a multipoint Brunauer-Emmett-Teller (BET)2(ii) in terms of/g. The pore size distribution in the embedded graph is obtained through NLDFT calculation, which shows that the pore size of the sample is mainly distributed between 0.6 nm and 1.9nm, and a small amount of pore sizes are between 42 nm and 55nm, and further proves that the material mainly has micropores and has a porous structure with coexisting mesopores and macropores.
The adsorption curve of the nitrogen-containing porous carbon material prepared according to the example 1 on the methyl orange solution is shown in fig. 3, from which the maximum adsorption capacity on the methyl orange can be derived to be 755.18 mg/g.
Comparative example
Methyl orange adsorption experiments of the nitrogen-containing porous carbon material (CN 1) prepared in this example 1 and commercial activated carbon powder (analytically pure, wind boat chemical reagent science co ltd, tianjin city, chemical reagent three works), activated carbon particles (analytically pure, wind boat chemical reagent science co ltd, tianjin city, chemical reagent three works):
20 mg of each of the nitrogen-containing porous carbon material (CN 1), activated carbon particles (AC-particle) and activated carbon Powder (AC-Powder) prepared in example 1 was taken to prepare 3 parts of a methyl orange solution having a concentration of 50 mg/L and a volume of 350 mL. Subsequently, 3 materials were put into 3 parts of methyl orange solution, and stirred at room temperature (24.6 ℃) for 24 hours. Before adding the sample, 0 h of initial solution is taken, then 1.5 ml of filtrate is taken at intervals of 2h, 6h, 12h and 24 h, diluted by 4 times, and the concentration of methyl orange in the solution is tested by an ultraviolet-visible spectrophotometer, so that the corresponding adsorption amount is calculated.
Results and analysis: the comparative graph of the adsorption curve for the methyl orange solution is shown in fig. 4.
Under the same experimental conditions, the commercial activated carbon powder has a faster adsorption rate on methyl orange, the adsorption capacity reaches 247.25 mg/g after 2 hours, then the adsorption equilibrium is gradually reached, and the adsorption capacity reaches 257.21 mg/g after 24 hours; the adsorption effect of the commercial activated carbon particles is relatively poor, and the adsorption capacity of 24 h is only 26.52 mg/g; the adsorption of the nitrogen-containing porous carbon material (CN 1) prepared in the example 1 on methyl orange is in a relatively rapid increasing trend, the adsorption capacity in 2 hours can reach 294.30 mg/g, and the adsorption capacity in 24 hours is 755.18 mg/g. This shows that the nitrogen-containing porous carbon material prepared in this example 1 has a better methyl orange adsorption performance than commercial activated carbon, and has a good application potential.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (3)
1. A preparation method of nitrogen-containing porous carbon based on jute is characterized by comprising the following steps:
(1) cutting and cleaning a sample: taking the length and width of 5cm multiplied by 2cm and the gram weight of 669.4g/m2Soaking a plurality of jute cloth strips in deionized water and ethanol respectively for ultrasonic treatment, washing for 10min at ultrasonic power of 150W and ultrasonic frequency of 60kHz, and drying in a blast drying oven at 80 ℃ for 12 h;
(2) loading an activating agent and a nitrogen-containing precursor: preparing 50mL of 1.5mol/L solution from 13.8170g of potassium oxalate crystals, and adding 0.1336g of urea into the solution; then, soaking 0.6681g of 2 pieces of dried jute cloth strips in the solution, taking the jute cloth strips out after 12h, and drying in an oven at 80 ℃ for 12 h;
(3) high-temperature carbonization: putting the loaded jute cloth strips into a corundum crucible, then putting the corundum crucible into a tubular furnace, vacuumizing the air in the tubular furnace for 10min by using a circulating water type vacuum pump, then introducing nitrogen as protective gas, wherein the flow rate is 25mL/min, setting the program to carry out high-temperature carbonization, the initial temperature is 25 ℃, the carbonization setting temperature is 700 ℃, the temperature is increased by 5 ℃ per minute, keeping the temperature for 2h when the temperature is increased to 700 ℃, then reducing the temperature to the room temperature at the speed of 3.7 ℃/min, and taking out a sample after the temperature is 80 ℃ to obtain the nitrogen-containing porous carbon material;
(4) washing and drying: soaking and washing the obtained carbonized sample for 3 times by using 30mL of dilute hydrochloric acid with the concentration of 1mol/L, soaking and washing the carbonized sample by using deionized water until the pH value is close to 7, and finally drying the carbonized sample in an oven at 80 ℃ for 12 hours for later use;
the maximum adsorption capacity of the nitrogen-containing porous carbon to methyl orange is 755.18 mg/g.
2. The nitrogen-containing porous carbon produced by the production method according to claim 1.
3. Use of the nitrogen-containing porous carbon of claim 2 for the mass adsorption of methyl orange.
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| CN113149006B (en) * | 2021-05-12 | 2021-11-02 | 广西科学院 | Method for preparing capacitance carbon by using biomass rich in lignin as raw material |
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