CN113415802A - Method for preparing carbon material by taking folium artemisiae argyi as raw material in low-temperature air atmosphere and application - Google Patents

Method for preparing carbon material by taking folium artemisiae argyi as raw material in low-temperature air atmosphere and application Download PDF

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CN113415802A
CN113415802A CN202110771295.2A CN202110771295A CN113415802A CN 113415802 A CN113415802 A CN 113415802A CN 202110771295 A CN202110771295 A CN 202110771295A CN 113415802 A CN113415802 A CN 113415802A
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folium artemisiae
artemisiae argyi
low
temperature
activating agent
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杨冉
曾华金
洪梦茹
屈凌波
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Zhengzhou University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention provides a method for preparing a carbon material by taking folium artemisiae argyi as a raw material in a low-temperature air atmosphere and application. The prepared carbon material has better oxidation resistance, adsorption performance and bacteriostasis performance compared with the wormwood waste material. The invention provides a new excellent choice for the comprehensive utilization of wormwood and wormwood waste and the development of high value-added wormwood material products, and provides a reference and basis of methodology for the simple and convenient preparation of low-cost biomass charcoal materials.

Description

Method for preparing carbon material by taking folium artemisiae argyi as raw material in low-temperature air atmosphere and application
Technical Field
The invention relates to the field of carbon nano materials, in particular to a method for preparing a carbon material by taking folium artemisiae argyi as a raw material in a low-temperature air atmosphere and application of the carbon material.
Background
The wormwood is a herbaceous plant with strong adaptability and capable of growing except extremely arid and alpine regions, is rich in various active ingredients such as volatile oil, flavone and tannic acid, and has the effects of sterilization, oxidation resistance, inflammation diminishing, cancer resistance and the like. The effect of the moxa is mainly used for preparing moxa sticks, the annual output value of the moxa-moxibustion market in China is nearly three billion, and the annual output value of the moxa-moxibustion is increased at a speed of 30-50%. In the process of making moxa sticks, nearly four fifths of the moxa leaves become waste.
The biomass charcoal material has the advantages of wide source, low cost, excellent physical and chemical properties and the like, and has good application prospect in the fields of wastewater treatment and adsorption, chemical industry, food and drug processing and energy storage materials. The traditional preparation of activated carbon material generally comprises the following steps: firstly, non-carbon atoms are removed under the protection of high-temperature (400-900 ℃) nitrogen, and then under the high-temperature condition, the oxidation of edge carbon atoms is carried out to obtain active groups with active reaction characteristics. High-temperature energy consumption in the preparation process and harsh nitrogen protection measures are required, which is not favorable for broad-spectrum popularization and has higher preparation cost.
Aiming at the problems that a large amount of wormwood waste materials are generated in the development process of the wormwood industry in China at present, high-temperature energy consumption is generated in the preparation process of biomass activated carbon, and the process is not beneficial to popularization and promotion, the preparation research of the biomass carbon materials is carried out in the low-temperature air atmosphere, the biomass materials with the performances of oxidation resistance, pollutant adsorption, bacteriostasis and the like are obtained, and a new excellent choice is provided for comprehensive utilization of the wormwood and the wormwood waste materials and development of high-value-added wormwood material products.
Disclosure of Invention
The invention provides a method for preparing a carbon material by taking folium artemisiae argyi as a raw material in a low-temperature air atmosphere, the method is used for preparing the carbon material in an air atmosphere at the temperature lower than 300 ℃, and the prepared carbon material has better oxidation resistance, adsorption performance and antibacterial performance compared with folium artemisiae argyi waste.
The technical scheme for realizing the invention is as follows:
a method for preparing a carbon material by taking folium artemisiae argyi as a raw material in a low-temperature air atmosphere comprises the following steps: folium artemisiae argyi is used as a raw material, an activating agent is added after pre-carbonization, stirring is carried out, cooling is carried out after low-temperature carbonization, and folium artemisiae argyi charcoal is obtained through washing, centrifuging and drying.
The activating agent is K2CO3The solution, acetic acid solution, mixed solution of potassium carbonate and hydrogen peroxide and mixed solution of acetic acid and hydrogen peroxide, and the concentration of the activating agent is 0.2-0.4 mol.L-1。
The temperature of the folium artemisiae argyi pre-carbonization is 220-250 ℃, and the time is 15 min.
The mass-volume ratio of the pre-carbonized folium artemisiae argyi to the activating agent is 1:8, and the stirring time is 4-6 h.
The low-temperature carbonization temperature is 280-300 ℃, and the time is 75 min.
Pre-carbonizing folium Artemisiae Argyi in a resistance furnace, adding activating agent at a certain proportion, stirring, carbonizing in an electric furnace, cooling to room temperature, washing with distilled water, centrifuging until the pH of the purified solution is neutral, and drying in an oven to obtain folium Artemisiae Argyi charcoal.
The Ehrlich carbon has a hollow structure, uniform pores and a graphene-like lamellar structure, and has a specific surface area of 3.39 m2·g-1Total pore volume of 0.013 cm3·g-1。
Preferably, the carbon material prepared by the invention is applied to free radical scavenging, bacteriostasis and wastewater cationic dye pollutant adsorption.
The invention has the beneficial effects that:
(1) compared with the reported preparation method of the biomass carbon material, the method is carried out at low temperature of 280 ℃ and in an air atmosphere without nitrogen protection, and has simple process and low energy consumption;
(2) compared with the mugwort, the prepared mugwort charcoal material has higher oxidation resistance;
(3) the prepared moxa charcoal material has a good bacteriostatic effect;
(4) the prepared mugwort charcoal material has stronger cationic dye adsorption performance compared with mugwort;
(5) the prepared mugwort charcoal material can be recycled after organic dye adsorption.
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 present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a TEM of the moxa carbon prepared in example 1.
FIG. 2 is an SEM of the moxa carbon prepared in example 1.
FIG. 3 is the adsorption curve of the moxa for cationic dyes of example 1.
FIG. 4 shows the cyclic regeneration capacity of the moxa for cationic dye adsorption of example 1 (m =10mg, MB =0.5 mg. multidot.ml)-1, pH~9）。
FIG. 5 is a comparison of dye adsorption capacity of the moxa charcoal of example 1 and that of mugwort grass.
FIG. 6 is EPR spectra of mugwort charcoal and mugwort in example 1.
FIG. 7 shows the OH radical removing ability of the Ehrlich carbon of example 1.
FIG. 8 is a graph showing the DPPH radical removal ability of the apyrocarbon of example 1.
FIG. 9 shows the ability of the Airbus char of example 1 to remove ABTS radicals.
FIG. 10 shows the bacteriostatic activity of the moxa charcoal of example 1, (a) E.coli; (b) staphylococcus aureus.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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 effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The specific synthetic steps of the moxa charcoal are as follows:
first, Artemisia princeps Pampanini (5g) was pre-carbonized (235 ℃ C., 15min) in an electric furnace (SX2-4-10A) to obtain 4.2g of a pre-carbonized carbon material. Secondly, adding an activating agent (K) according to a certain ratio (1:8)2CO3, 0.2mol·L-1) And stirring for 5 hours. Finally, charring on an electric furnace (280 ℃, 75min), cooling to room temperature, washing with distilled water, and centrifuging until the pH of the purified solution is neutral. Drying in an oven at 100 deg.C for 8 hr, and taking out to obtain folium Artemisiae Argyi charcoal (MC).
As can be seen in fig. 2(a), MC retains the fibrous nature of the raw material; fig. 2(b) shows that MC has uniform pores. TEM images according to fig. 1(c) and (d) show that MC has a graphene-like lamellar structure.
Example 2
The specific synthetic steps of the moxa charcoal are as follows:
first, Artemisia princeps Pampanini (5g) was pre-carbonized (220 ℃ C., 15min) in an electric furnace (SX2-4-10A) to obtain 4.2g of a pre-carbonized carbon material. Secondly, adding an activating agent (a mixed solution of potassium carbonate and hydrogen peroxide, 0.3 mol. L) according to a certain ratio (1:8)-1) And stirring for 5 hours. Finally, charring on an electric furnace (290 ℃, 75min), cooling to room temperature, washing with distilled water, and centrifuging until the pH of the purified solution is neutral. Drying in an oven at 100 deg.C for 8 hr, and taking out to obtain folium Artemisiae Argyi charcoal (MC).
Example 3
The specific synthetic steps of the moxa charcoal are as follows:
first, Artemisia princeps Pampanini (5g) was pre-carbonized (250 ℃ C., 15min) in an electric furnace (SX2-4-10A) to obtain 4.2g of a pre-carbonized carbon material. Secondly, an activating agent (acetic acid solution, 0.4 mol. L) is added according to a certain proportion (1:8)-1) And stirring for 5 hours. Finally, charring on an electric furnace (300 ℃, 75min), cooling to room temperature, washing with distilled water, and centrifuging until the pH of the purified solution is neutral. Drying in an oven at 100 deg.C for 8h, and taking out to obtainCharred folium Artemisiae Argyi (MC).
Performance study was conducted using the moxa carbon prepared in example 1
(1) Adsorption experiment of Ehrlich carbon to methylene blue
In order to analyze the adsorption phenomenon and understand the adsorption type, the adsorption isotherm is explored. Nonlinear fitting was performed by three models, Freundlich, Langmuir and Koble-Corrigan. 10mg MC and 10mL of 0.18 mg. multidot.mL were added to a series of 50 mL Erlenmeyer flasks-1~0.5 mg·mL-1The MB of (1). Shaking at 293 k, 303 k, 313 k for 360 min (120 rpm).
As can be seen from fig. 3, when the temperature is constant, the unit adsorption amount of MC gradually increases as the equilibrium concentration increases. This is primarily due to the relatively large number of MBs surrounding a unit area of the adsorbent as the concentration of MBs increases, resulting in a large number of MBs that can be bound by the active sites of the adsorbent. As the concentration of MB increases, the active sites of the adsorbent are gradually occupied, thereby gradually saturating the adsorption; due to the concentration difference of the methylene blue solution, the concentration of MB is increased, and the adsorption capacity is still increased. It can be seen from fig. 3 that the adsorption amount gradually increases with the increase of the temperature, which indicates that the adsorption process of MC to MB is an endothermic process.
(2) Cyclic regeneration of moxa charcoal
Placing the adsorbed folium Artemisiae Argyi charcoal in an electric furnace (235 deg.C, 15min), activating and carbonizing. And then putting the regenerated moxa charcoal (10 mg) into 10ml of methylene blue solution (0.5 mg/ml pH-9). After the adsorption equilibrium, the reusability of the nano-moxa carbon was determined by measuring the adsorption capacity.
As can be seen from fig. 4, even when three cycles of regeneration were achieved, the adsorption capacity of the adsorbent remained balanced, indicating that the adsorbent had good regeneration capacity.
(3) EPR scanning of Airbus carbon and Airbus
Weighing the moxa carbon powder and the moxa powder with the same amount, putting the materials into a nuclear magnetic tube, and measuring the EPR (ethylene-propylene-diene monomer) spectrum of the materials on an electronic self-selected resonance instrument.
(4) Ability of moxa charcoal to remove free radicals
10mg of moxa carbon is weighed, 3ml of water is added, after the moxa carbon is soaked for 2 hours, the obtained mixture is centrifuged, and supernatant fluid is obtained for carrying out the anti-free radical experiment. FIG. 5 Elaeagnus charcoal for DPPH radical scavenging. The same fig. 6 shows the ABTS removal by the moxa charcoal.
(5) Antibacterial activity of mugwort charcoal
By a plate counting method, representative gram-negative bacteria escherichia coli and gram-positive bacteria staphylococcus aureus are selected, and the antibacterial performance of BAC is researched. Colonies were first placed in sterilized liquid medium (5 mL) and incubated for 18 h at 37 ℃ on a shaker. Centrifuging the cultured bacterial suspension at 5000 rpm for 5min, and washing with 1 × PBS buffer solution for 3 times; after washing, the cells were resuspended in 1 XPBS buffer and diluted to OD600= 0.5; 1 mL of the bacterial solution (OD)600= 0.5) add 0.01 g BAC, shake for 1 h at 37 ℃; after completion, the bacterial suspension was serially diluted 1X 10 with 1 XPBS buffer5Doubling; and transferring 100 mu l of the diluted bacterial suspension into a solid culture medium, uniformly coating the solid culture medium by using a coating rod, and culturing for 18 h at 37 ℃. The percentage of viable bacteria was calculated from the number of colonies formed, the dilution factor and the sample size.
As can be seen from fig. 10, the inhibition rates of MC on staphylococcus aureus and escherichia coli are 91.38% and 30.60%, respectively, and thus it can be seen that MC has a good bacteriostatic effect on staphylococcus aureus. The isoelectric point of MC is about 7.5, the pH buffered by PBS is 7.4, the pH value in the solution is not greatly different from the isoelectric point, and a small amount of charges on the surface of MC can not have significant influence on bacteriostasis.
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 (8)

1. A method for preparing a carbon material by taking folium artemisiae argyi as a raw material in a low-temperature air atmosphere is characterized by comprising the following steps: folium artemisiae argyi is used as a raw material, an activating agent is added after pre-carbonization, stirring is carried out, cooling is carried out after low-temperature carbonization, and folium artemisiae argyi charcoal is obtained through washing, centrifuging and drying.
2. The method of claim 1, wherein: the activating agent is K2CO3The solution, acetic acid solution, mixed solution of potassium carbonate and hydrogen peroxide and mixed solution of acetic acid and hydrogen peroxide, and the concentration of the activating agent is 0.2-0.4 mol.L-1。
3. The method of claim 1, wherein: the temperature of the folium artemisiae argyi pre-carbonization is 220-250 ℃, and the time is 15 min.
4. The method of claim 1, wherein: the mass-volume ratio of the pre-carbonized folium artemisiae argyi to the activating agent is 1:8, and the stirring time is 4-6 h.
5. The method of claim 1, wherein: the low-temperature carbonization temperature is 280-300 ℃, and the time is 75 min.
6. The method according to any one of claims 1 to 5, wherein: pre-carbonizing folium Artemisiae Argyi in a resistance furnace, adding activating agent at a certain proportion, stirring, carbonizing in an electric furnace, cooling to room temperature, washing with distilled water, centrifuging until the pH of the purified solution is neutral, and drying in an oven to obtain folium Artemisiae Argyi charcoal.
7. The method of claim 6, wherein: the Ehrlich carbon has a hollow structure, uniform pores and a graphene-like lamellar structure, and has a specific surface area of 3.39 m2·g-1Total pore volume of 0.013 cm3·g-1。
8. Use of the carbon material prepared by the method of claim 6 for radical scavenging, bacteriostasis and adsorption of cationic dye contaminants from wastewater.
CN202110771295.2A 2021-07-08 2021-07-08 Method for preparing carbon material by taking folium artemisiae argyi as raw material in low-temperature air atmosphere and application Pending CN113415802A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116162455A (en) * 2023-01-06 2023-05-26 黄冈师范学院 Moxa smoke carbon dot and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108217647A (en) * 2018-01-26 2018-06-29 上海理工大学 A kind of wormwood based biomass activated carbon and preparation method thereof and its application
CN108423675A (en) * 2018-03-02 2018-08-21 河南工程学院 The preparation method of high adsorption rate activated carbon
CN110092379A (en) * 2019-04-12 2019-08-06 蚌埠学院 It is a kind of using biomass as the method and application of raw material one-step synthesis sulfonation active carbon

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108217647A (en) * 2018-01-26 2018-06-29 上海理工大学 A kind of wormwood based biomass activated carbon and preparation method thereof and its application
CN108423675A (en) * 2018-03-02 2018-08-21 河南工程学院 The preparation method of high adsorption rate activated carbon
CN110092379A (en) * 2019-04-12 2019-08-06 蚌埠学院 It is a kind of using biomass as the method and application of raw material one-step synthesis sulfonation active carbon

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116162455A (en) * 2023-01-06 2023-05-26 黄冈师范学院 Moxa smoke carbon dot and preparation method and application thereof
CN116162455B (en) * 2023-01-06 2023-11-21 黄冈师范学院 Moxa smoke carbon dot and preparation method and application thereof

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