CN114950360A - Biomass activated carbon adsorption material derived from lotus leaves and preparation method and application thereof - Google Patents
Biomass activated carbon adsorption material derived from lotus leaves and preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 240000002853 Nelumbo nucifera Species 0.000 title claims abstract description 68
- 235000006508 Nelumbo nucifera Nutrition 0.000 title claims abstract description 68
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- 239000000463 material Substances 0.000 title claims abstract description 56
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 46
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B01J2220/48—Sorbents characterised by the starting material used for their preparation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention discloses a biomass activated carbon adsorption material derived from lotus leaves and a preparation method and application thereof, wherein the method comprises the following steps: drying and crushing lotus leaves to obtain lotus leaf powder; calcining the lotus leaf powder in a nitrogen atmosphere for one time to obtain lotus leaf carbon; ball-milling the lotus leaf carbon to obtain a precursor; uniformly mixing the precursor and zinc chloride solids, adding deionized water, carrying out oil bath stirring, washing and drying to obtain a modified precursor; and grinding the modified precursor, and then carrying out secondary calcination in a nitrogen atmosphere to obtain the biomass activated carbon material. The prepared activated carbon has larger specific surface area and abundant pore structures, and can effectively remove dyes and antibiotics in water.
Description
Technical Field
The invention relates to the technical field of adsorbing materials, in particular to a biomass activated carbon adsorbing material derived from lotus leaves and a preparation method and application thereof.
Background
Waste water produced by the textile industry is a common pollution problem worldwide, and among textile waste water, the degradation of dye waste water is most difficult. However, these dye waste water which is difficult to degrade often threatens environment pollution and human health, the dye is resistant to photodegradation and strong in oxidation resistance, and can absorb light to cause the transparency of the water body to be reduced, thereby influencing the photosynthesis of organisms such as algae, leading to the death of the organisms and destroying the ecological balance of the water body. In addition, the dyes are often biotoxic or denaturalized, which not only poison aquatic organisms, but also have great threat to human health.
Antibiotics are used as specific drugs for treating infectious diseases, but serious environmental risks are caused by abuse of the antibiotics, 5% -90% of the antibiotics are not metabolized after entering a human body or an animal body and are discharged out of the body along with urine or feces, the antibiotics are discharged for a long time and directly or indirectly enter an environmental water body to cause enhancement of drug resistance of sensitive bacteria, and drug resistance genes can expand and evolve in the environment, so that serious threats are caused to ecological environment and human health.
In order to build a better ecological environment and reduce the pollution condition of dye and antibiotic to the water environment, the preparation of a good adsorption material is an urgent need, and the prior wastewater treatment method comprises a chemical coagulation method, a biological method, an adsorption method, an oxidation method and the like. The adsorption method has the characteristics of low cost, simple operation and high efficiency, and has very wide industrial application prospect. Activated carbon is widely applied as an efficient adsorbent, but the activated carbon is generally prepared by high-temperature calcination of high-quality coal or petroleum coke and other carbon-containing raw materials and is relatively expensive, and biomass activated carbon is widely concerned as a new clean carbon source due to low cost, wide sources and sustainability.
Therefore, there is an urgent need to develop a biomass activated carbon material that can effectively remove dyes and antibiotics from water.
Disclosure of Invention
The invention aims to provide a biomass activated carbon adsorption material derived from lotus leaves and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a method for preparing a biomass activated carbon adsorbent material derived from lotus leaves, the method comprising:
drying and crushing lotus leaves to obtain lotus leaf powder;
calcining the lotus leaf powder in a nitrogen atmosphere for one time to obtain lotus leaf carbon;
ball-milling the lotus leaf carbon to obtain a precursor;
uniformly mixing the precursor and zinc chloride solids, adding deionized water, carrying out oil bath stirring, washing and drying to obtain a modified precursor;
and grinding the modified precursor, and then carrying out secondary calcination in a nitrogen atmosphere to obtain the biomass activated carbon material.
Further, the conditions of the primary calcination are as follows: calcining for 1-3 h at the temperature of 750-850 ℃ at the temperature rising rate of 4-6 ℃/min, wherein N is 2 The flow rate is 35-45 mL/min.
Further, the rotation speed of the ball milling is 110-130 rpm/min, and the ball milling time is 1-3 h.
Further, the mass ratio of the precursor to the zinc chloride solid is 1: (1-3).
Further, the stirring temperature of the oil bath is 65-75 ℃, the stirring speed of the oil bath is 250-350 rpm, and the stirring time of the oil bath is 5-7 hours.
Further, the temperature of the drying treatment is 65-75 ℃.
Further, the conditions of the secondary calcination are as follows: calcining at the temperature of 700-900 ℃ for 0.5-2 h at the temperature rising rate of 8-12 ℃/min, and N 2 The flow rate is 35-45 mL/min.
In a second aspect of the invention, a biomass activated carbon adsorption material derived from lotus leaves prepared by the method is provided.
In a third aspect of the invention, the application of the biomass activated carbon adsorbing material derived from lotus leaves in removing dyes and/or antibiotics in water is provided.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the embodiment of the invention provides a biomass activated carbon adsorption material derived from lotus leaves and a preparation method and application thereof 2 The modification and the high-temperature calcination are carried out, so that the adsorbing material has the advantages of low price, reproducibility and high specific surface area, and the reproducibility and the high specific surface area are favorable for the preparation and the performance improvement of the adsorbing material.
Compared with the traditional method for preparing the activated carbon, the method has the advantages of lower price, no pollution, reproducibility and wide source, compared with the activated carbon material obtained by simply calcining biomass, the activated carbon prepared by the preparation method has larger specific surface area and abundant pore structures, can effectively remove dyes and antibiotics in water, and specifically comprises the following steps: preparing a bottle of methyl orange solution with the concentration of 50mg/L and norfloxacin solution with the concentration of 30mg/L for later use, respectively taking 100mL of each solution from the two bottles, transferring the solution into a conical flask, taking 0.02g of LAC-2-900 biomass carbon material out, respectively adding the material into the two conical flasks, placing a beaker filled with the adsorbent and the solution into a temperature-controlled shaking table, stirring at the stirring speed of 200rpm/min, and testing the adsorption performance of the beaker by using a UV-2600i ultraviolet spectrophotometer. The LAC-2-900 sample has an adsorption capacity of 162mg/g in 5h and 63mg/g in norfloxacin adsorption when adsorbing methyl orange solution.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is an X-ray diffraction pattern of activated carbon materials prepared in example 5 of the present invention and comparative example 1.
Fig. 2 is a graph showing the adsorption performance of methyl orange solutions adsorbed in example 1, example 2, example 3, example 4, example 5, and comparative example 1 of the present invention.
Fig. 3 is a graph showing adsorption performance of norfloxacin solutions adsorbed in examples 1, 2, 3, 4, 5 and 1 of the present invention.
Fig. 4 is an adsorption isotherm curve for adsorbing methyl orange solutions at different concentrations in example 1, example 2, example 3, example 4, example 5, and comparative example 1 of the present invention.
Fig. 5 is adsorption isotherms of norfloxacin solutions at different concentrations according to example 1, example 2, example 3, example 4, example 5, and comparative example 1 of the present invention.
FIG. 6 is a scanning electron micrograph of an activated carbon material prepared in example 5 of the present invention and comparative example 1; wherein fig. 6(a) and 6(b) are sem images of the activated carbon material prepared in comparative example 1, and fig. 6(c) and 6(d) are sem images of the activated carbon material prepared in example 5.
Fig. 7 is a nitrogen adsorption/desorption graph of examples 1, 2, 3, 4, 5 and 1 of the present invention.
FIG. 8 is a flow chart of a method for preparing a biomass activated carbon adsorbent material derived from lotus leaf according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are illustrative of the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be obtained by an existing method.
The general idea of the invention is as follows:
according to an exemplary embodiment of the present invention, there is provided a method for preparing a biomass activated carbon adsorption material derived from lotus leaves, the method including:
step S1, drying and crushing lotus leaves to obtain lotus leaf powder;
in the step S1, in the above step,
the drying can be carried out in an electrothermal blowing drying oven, and the drying temperature is 65-70 ℃;
step S2, calcining the lotus leaf powder in a nitrogen atmosphere to obtain lotus leaf carbon;
in the above technical scheme, the conditions of the primary calcination are as follows: calcining for 1-3 h at the temperature of 750-850 ℃ at the temperature rising rate of 4-6 ℃/min, wherein N is 2 The flow rate is 35-45 mL/min.
If the temperature rise rate is too high, the reaction is too violent, the agglomeration phenomenon is serious, and if the temperature rise rate is too low, the energy consumption is too high;
if the calcination temperature is too high, the yield of the carbon material is too low, the internal pore structure of the carbon material collapses, and if the calcination temperature is too low, a large specific surface area is not generated, and a large amount of aromatic substances are not volatilized;
said N is 2 If the flow is too large, the sample can be carried out, and if the flow is too small, external air can enter the tube furnace, so that adverse effects are generated;
s3, performing ball milling on the lotus leaf carbon to obtain a precursor;
in the technical proposal mentioned above, the method comprises the following steps,
the rotation speed of the ball milling is 110-130 rpm/min, and the ball milling time is 1-3 h. The ball milling condition is favorable for reducing the particle size of the lotus leaf carbon, and can not greatly influence the original structure of the lotus leaf carbon.
Step S4, uniformly mixing the precursor and the zinc chloride solid, adding deionized water, carrying out oil bath stirring, washing and drying to obtain a modified precursor;
the mass ratio of the precursor to the zinc chloride solid is 1: (1-3); the effect of the adsorbent obtained in this mass ratio is superior, and the mass ratio is preferably 1: 2; the adsorption material has the most excellent effect; if the mass ratio is too small, namely the zinc chloride solid is added too much, the excessive zinc chloride can block the pore channel structure and is not beneficial to adsorption; if the mass ratio is too large, namely the addition of zinc chloride solids is too little, the activation is insufficient;
the stirring temperature of the oil bath is 65-75 ℃, the stirring speed of the oil bath is 250-350 rpm, and the stirring time of the oil bath is 5-7 h. The oil bath condition is favorable for accelerating the molecular thermal motion, so that the activation time is greatly shortened, and the activation is sufficient.
The temperature of the drying treatment is 65-75 ℃.
And step S5, grinding the modified precursor, and then carrying out secondary calcination in a nitrogen atmosphere to obtain the biomass activated carbon material.
The conditions of the secondary calcination are as follows: calcining at the temperature of 700-900 ℃ for 0.5-2 h at the temperature rising rate of 8-12 ℃/min, and N 2 The flow rate is 35-45 mL/min.
The heating rate and the calcining temperature of the secondary calcining are both larger than those of the primary calcining,
if the temperature rise rate is too high, the reaction is too violent, the agglomeration phenomenon is serious, and if the temperature rise rate is too low, the energy consumption is too high;
if the calcination temperature is too high, the internal pore structure of the carbon material can collapse, and if the calcination temperature is too low, the specific surface area is not increased;
said N is 2 If the flow rate is too large, the sample can be carried out, and if the flow rate is too small, external air can enter the interior of the tube furnace, so that adverse effects are generated;
the invention also provides the biomass activated carbon adsorbing material derived from the lotus leaves, which is prepared by the method.
The invention also provides application of the biomass activated carbon adsorption material derived from lotus leaves in removing dyes and/or antibiotics in water.
The following will explain in detail a biomass activated carbon adsorbing material derived from lotus leaves, its preparation method and application in the present application with reference to examples and experimental data.
Example 1 Biomass activated carbon adsorption Material derived from Lotus leaf and method for preparing the same
(1) Pulverizing certain amount of folium Nelumbinis into powder in a pulverizer, transferring the pulverized granules into an electrothermal blowing drying oven, drying at 70 deg.C, collecting small amount of folium Nelumbinis powder, placing into a tubular furnace, and introducing N 2 The flow is 40mL/min, the lotus leaf carbon is heated to 800 ℃ at the heating rate of 5 ℃/min and kept for 2h, the burnt carbon is taken out after natural cooling, a certain amount of the burnt carbon is put into a planetary ball mill and is ball-milled for 2h at the rotating speed of 120rpm/min, and the ball-milled product is collected to obtain the lotus leaf carbon prepared by primary calcination as a precursor LC.
(2) Taking out 1g of the precursor, pouring the precursor into a beaker, adding 1g of zinc chloride solid particles into the beaker, pouring 17mL of deionized water solution into the beaker, placing the beaker into a temperature-controlled magnetic stirrer, magnetically stirring at 200rpm/min and stirring at 70 ℃ for 6 hours to obtain a zinc chloride activated carbohydrate suspension, then repeatedly washing with deionized water for more than 7 times through operations such as washing, centrifuging and the like in sequence, and then repeatedly washing with deionized water for more than 7 timesAnd (3) placing the obtained solid product in an electric heating forced air drying oven, and drying at 70 ℃ to obtain the activated lotus leaf carbon material. Loading the activated carbon material of lotus leaf into a tube furnace, and introducing N 2 The flow rate is 40mL/min, the temperature is raised to 700 ℃ at the heating rate of 10 ℃/min and is kept for 1h, and after natural cooling, the burnt carbon is collected, so that the LAC-1-700 activated carbon material is obtained.
Example 2
In this example, except for the different addition ratios of the zinc chloride solid, the other examples were the same as example 1, specifically:
(1) pulverizing certain amount of folium Nelumbinis into powder in a pulverizer, transferring the pulverized granules into an electrothermal blowing drying oven, drying at 70 deg.C, collecting small amount of folium Nelumbinis powder, placing into a tubular furnace, and introducing N 2 The flow is 40mL/min, the lotus leaf carbon is heated to 800 ℃ at the heating rate of 5 ℃/min and kept for 2h, the burnt carbon is taken out after natural cooling, a certain amount of the burnt carbon is put into a planetary ball mill and is ball-milled for 2h at the rotating speed of 120rpm/min, and the ball-milled product is collected to obtain the lotus leaf carbon prepared by primary calcination as a precursor LC.
(2) And taking 1g of the precursor out, pouring into a beaker, adding 3g of zinc chloride solid particles into the beaker, pouring 17mL of deionized water solution, placing the beaker into a temperature-controlled magnetic stirrer, magnetically stirring at 200rpm/min and stirring at 70 ℃ for 6h to obtain a zinc chloride activated carbohydrate suspension, sequentially carrying out operations such as washing, centrifuging and the like, repeatedly washing with deionized water for more than 7 times, then placing the obtained solid product into an electrothermal blowing drying box, and drying at 70 ℃ to obtain the activated lotus leaf carbon material. And (2) filling the activated lotus leaf carbon material into a tubular furnace, introducing N2 with the flow rate of 40mL/min, heating to 700 ℃ at the heating rate of 10 ℃/min, keeping for 1h, and collecting the burnt carbon after natural cooling to obtain the LAC-3-700 activated carbon material.
Example 3
In this example, except for the different addition ratios of the zinc chloride solid, the other examples were the same as example 1, specifically:
(1)pulverizing certain amount of folium Nelumbinis into powder in a pulverizer, transferring the pulverized granules into an electrothermal blowing drying oven, drying at 70 deg.C, collecting small amount of folium Nelumbinis powder, placing into a tubular furnace, and introducing N 2 The flow is 40mL/min, the lotus leaf carbon is heated to 800 ℃ at the heating rate of 5 ℃/min and kept for 2h, the burnt carbon is taken out after natural cooling, a certain amount of the burnt carbon is put into a planetary ball mill and is ball-milled for 2h at the rotating speed of 120rpm/min, and the ball-milled product is collected to obtain the lotus leaf carbon prepared by primary calcination as a precursor LC.
(2) And taking 1g of the precursor out, pouring into a beaker, adding 2g of zinc chloride solid particles into the beaker, pouring 17mL of deionized water solution, placing the beaker into a temperature-controlled magnetic stirrer, magnetically stirring at 200rpm/min and stirring at 70 ℃ for 6h to obtain a zinc chloride activated carbohydrate suspension, sequentially carrying out operations such as washing, centrifuging and the like, repeatedly washing with deionized water for more than 7 times, then placing the obtained solid product into an electrothermal blowing drying box, and drying at 70 ℃ to obtain the activated lotus leaf carbon material. Loading the activated carbon material of lotus leaf into a tube furnace, and introducing N 2 The flow rate is 40mL/min, the temperature is raised to 700 ℃ at the heating rate of 10 ℃/min and is kept for 1h, and after natural cooling, the burnt carbon is collected, so that the LAC-2-700 activated carbon material is obtained.
Example 4
In this example, the conditions of the secondary calcination were different from those of example 3, and the other steps were the same as those of example 3, specifically:
(1) pulverizing certain amount of folium Nelumbinis into powder in a pulverizer, transferring the pulverized granules into an electrothermal blowing drying oven, drying at 70 deg.C, collecting small amount of folium Nelumbinis powder, placing into a tubular furnace, and introducing N 2 The flow is 40mL/min, the lotus leaf carbon is heated to 800 ℃ at the heating rate of 5 ℃/min and kept for 2h, the burnt carbon is taken out after natural cooling, a certain amount of the burnt carbon is put into a planetary ball mill and is ball-milled for 2h at the rotating speed of 120rpm/min, and the ball-milled product is collected to obtain the lotus leaf carbon prepared by primary calcination as a precursor LC.
(2) And taking 1g of the precursor out, pouring into a beaker, adding 2g of zinc chloride solid particles into the beaker, pouring 17mL of deionized water solution, placing the beaker into a temperature-controlled magnetic stirrer, magnetically stirring at 200rpm/min and stirring at 70 ℃ for 6h to obtain a zinc chloride activated carbohydrate suspension, sequentially carrying out operations such as washing, centrifuging and the like, repeatedly washing with deionized water for more than 7 times, then placing the obtained solid product into an electrothermal blowing drying box, and drying at 70 ℃ to obtain the activated lotus leaf carbon material. Loading the activated carbon material of lotus leaf into a tube furnace, and introducing N 2 The flow rate is 40mL/min, the temperature is raised to 800 ℃ at the heating rate of 10 ℃/min and is kept for 1h, and after natural cooling, the burnt carbon is collected, so that the LAC-2-800 activated carbon material is obtained.
Example 5
In this example, the conditions of the secondary calcination were different from those of example 3, and the other steps were the same as those of example 3, specifically:
(1) pulverizing certain amount of folium Nelumbinis into powder in a pulverizer, transferring the pulverized granules into an electrothermal blowing drying oven, drying at 70 deg.C, collecting small amount of folium Nelumbinis powder, placing into a tubular furnace, and introducing N 2 The flow is 40mL/min, the lotus leaf carbon is heated to 800 ℃ at the heating rate of 5 ℃/min and kept for 2h, the burnt carbon is taken out after natural cooling, a certain amount of the burnt carbon is put into a planetary ball mill and is ball-milled for 2h at the rotating speed of 120rpm/min, and the ball-milled product is collected to obtain the lotus leaf carbon prepared by primary calcination as a precursor LC.
(2) And taking 1g of the precursor out, pouring into a beaker, adding 2g of zinc chloride solid particles into the beaker, pouring 17mL of deionized water solution, placing the beaker into a temperature-controlled magnetic stirrer, magnetically stirring at 200rpm/min and stirring at 70 ℃ for 6h to obtain a zinc chloride activated carbohydrate suspension, sequentially carrying out operations such as washing, centrifuging and the like, repeatedly washing with deionized water for more than 7 times, then placing the obtained solid product into an electrothermal blowing drying box, and drying at 70 ℃ to obtain the activated lotus leaf carbon material. Loading the activated carbon material of lotus leaf into a tube furnace, and introducing N 2 A flow rate ofHeating to 900 ℃ at the heating rate of 10 ℃/min for 1h at 40mL/min, and collecting the burnt carbon after natural cooling to obtain the LAC-2-900 activated carbon material.
Comparative example 1
The comparative example only carries out primary calcination, does not add zinc chloride and carries out secondary calcination, and specifically comprises the following steps:
pulverizing certain amount of folium Nelumbinis into powder in a pulverizer, transferring the pulverized granules into an electrothermal blowing drying oven, drying at 70 deg.C, collecting small amount of folium Nelumbinis powder, placing into a tubular furnace, and introducing N 2 The flow is 40mL/min, the lotus leaf carbon is heated to 800 ℃ at the heating rate of 5 ℃/min and kept for 2h, the burnt carbon is taken out after natural cooling, a certain amount of the burnt carbon is put into a planetary ball mill and is ball-milled for 2h at the rotating speed of 120rpm/min, and the ball-milled product is collected to obtain the lotus leaf carbon prepared by primary calcination as a precursor LC.
Experimental example 1, Performance test
The performance of each example and each comparative example is tested, and the specific surface area and the adsorption effect are shown in table 1;
the performance test method comprises the following steps: 100mL of 50mg/L methyl orange and 100mL of 30mg/L norfloxacin solution are measured and poured into a conical flask, 0.02g of each of the activated carbon materials obtained by the preparation method is added into the conical flask, the conical flask is placed into a temperature-controlled shaking table and is stirred for 5 hours with shaking at the rotating speed of 200rpm/min, during the stirring, a UV-2600i ultraviolet spectrophotometer is used for testing the change of the absorbance of the dye, and the adsorption capacity is obtained through calculation.
TABLE 1
From the data in table 1, it can be seen that:
compared with the comparative example 1, the adsorbing materials obtained in the examples 1 to 5 of the invention have larger surface areas and larger adsorbing amounts of methyl orange and norfloxacin.
Fig. 1 shows X-ray diffraction patterns of example 5 and comparative example 1, and it can be found that in example 5, broad peaks are shown at 2 θ ═ 24.8 ° and 2 θ ═ 42.9 °, indicating that the prepared activated carbon material mainly contains a large amount of amorphous carbon. The peak generated in comparative example 1 is formed by the substance contained in the biomass itself.
Fig. 2 is a graph of adsorption performance of biomass carbon prepared in examples 1, 2, 3, 4, and 5 for adsorbing methyl orange solution for 5h, and it can be clearly observed that all the examples have different degrees of performance improvement compared to comparative example 1, and the example 5 has the most obvious effect improvement, which is attributed to that the precursor is sufficiently activated by the most suitable salt impregnation ratio, and the higher secondary calcination temperature generates a richer pore structure therein, so that the specific surface area is greatly increased, and solute molecules are more favorably absorbed into the pore structure of activated carbon, and adsorption is more favorably achieved.
Fig. 3 is a graph of adsorption performance of the biomass carbon prepared in examples 1, 2, 3, 4 and 5 for adsorbing norfloxacin 5h, the adsorption effect of all the examples is similar to the trend of fig. 2, and the activated carbon material prepared by the method has a certain adsorption effect on different pollutants in water and has good applicability.
Fig. 4 and 5 are graphs showing the effects of example 1, example 2, example 3, example 4 and example 5 in adsorbing different concentrations of methyl orange and norfloxacin, respectively, and Langmuir and Freundlich are fitted to the adsorption curves to find that the adsorption process is suitable for the Langmuir adsorption isotherm.
In fig. 6, (a) and (b) are sem images of the activated carbon material prepared in comparative example 1, and (c) and (d) are sem images of the activated carbon material prepared in example 5, and it can be seen by comparison that the LC activated carbon material is formed by stacking relatively large particles before activation and secondary calcination, but the activated and secondary calcined LAC-2-900 activated carbon material can obviously show that the particle size is reduced, and the stacking between particles generates a mesoporous structure on the surface thereof (circled by a dotted line in the figure), which is beneficial for the contaminants to enter and be adsorbed in the pores, thereby enhancing the adsorption effect.
Fig. 7 shows the nitrogen adsorption and desorption curves of example 1, example 2, example 3, example 4, and example 5, respectively, from which the specific surface areas of the different examples were calculated by the BET equation, and the results are shown in table two. LAC-2-900 has the largest specific surface area reaching 682m 2 The results of the experiments in fig. 2 and 3 show that a larger specific surface area is more advantageous for increasing the adsorption effect.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including the preferred embodiment and all changes and modifications that fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. A preparation method of a biomass activated carbon adsorption material derived from lotus leaves is characterized by comprising the following steps:
drying and crushing lotus leaves to obtain lotus leaf powder;
calcining the lotus leaf powder in a nitrogen atmosphere for one time to obtain lotus leaf carbon;
ball-milling the lotus leaf carbon to obtain a precursor;
uniformly mixing the precursor and zinc chloride solids, adding deionized water, carrying out oil bath stirring, washing and drying to obtain a modified precursor;
and grinding the modified precursor, and then carrying out secondary calcination in a nitrogen atmosphere to obtain the biomass activated carbon material.
2. The method for preparing the biomass activated carbon adsorbing material derived from the lotus leaves as claimed in claim 1, wherein the conditions of the primary calcination are as follows: calcining for 1-3 h at the temperature of 750-850 ℃ at the temperature rising rate of 4-6 ℃/min, wherein N is 2 The flow rate is 35-45 mL/min.
3. The preparation method of the biomass activated carbon adsorbing material derived from lotus leaves as claimed in claim 1, wherein the rotation speed of the ball milling is 110-130 rpm/min, and the time of the ball milling is 1-3 h.
4. The preparation method of the biomass activated carbon adsorption material derived from lotus leaves as claimed in claim 1, wherein the mass ratio of the precursor to the zinc chloride solid is 1: (1-3).
5. The preparation method of the biomass activated carbon adsorption material derived from lotus leaves as claimed in claim 1, wherein the temperature of the oil bath stirring is 65-75 ℃, the speed of the oil bath stirring is 250-350 rpm, and the time of the oil bath stirring is 5-7 h.
6. The method for preparing the biomass activated carbon adsorbing material derived from the lotus leaves as claimed in claim 1, wherein the temperature of the drying treatment is 65-75 ℃.
7. The method for preparing the biomass activated carbon adsorbing material derived from the lotus leaves as claimed in claim 1, wherein the conditions of the secondary calcination are as follows: at 8-12 ℃Calcining at 700-900 ℃ for 0.5-2 h at the temperature rise rate of min, wherein N is 2 The flow rate is 35-45 mL/min.
8. A biomass activated carbon adsorbent material derived from lotus leaves, prepared by the method of any one of claims 1 to 7.
9. Use of a biomass activated carbon sorbent material derived from lotus leaf as claimed in claim 8 for the removal of dyes and/or antibiotics from water.
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