CN110817864A - Plant-based activated carbon and preparation method and application thereof - Google Patents
Plant-based activated carbon and preparation method and application thereof Download PDFInfo
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- CN110817864A CN110817864A CN201911157963.1A CN201911157963A CN110817864A CN 110817864 A CN110817864 A CN 110817864A CN 201911157963 A CN201911157963 A CN 201911157963A CN 110817864 A CN110817864 A CN 110817864A
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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
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- 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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
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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
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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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
-
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The invention relates to plant-based activated carbon and a preparation method and application thereof. The microstructure of the plant-based activated carbon is long tubular, the inside of the pipeline has rich pore diameter structures, the specific surface area is large, the antibiotic adsorption performance is good, especially the antibiotic adsorption performance with ultralow concentration is excellent, and the plant-based activated carbon can be used for adsorbing antibiotic pollutants. The plant selected by the invention is a common plant in the nature, the distribution field is wide, the large-scale preparation can be realized, the preparation method is simple, complex equipment is not needed, expensive reactants are not involved, the cost is low, the prepared plant-based activated carbon is used for adsorption, and the preparation method and the application field of the adsorption material can be expanded.
Description
Technical Field
The invention belongs to the field of preparation of green and environment-friendly materials, and particularly relates to plant-based activated carbon and a preparation method and application thereof.
Background
The activated carbon is an important porous material, and is an adsorbent which is widely applied and has good economical efficiency due to the characteristics of large specific surface area, developed pore-size structure, stable physicochemical property, high mechanical strength, rich sources, easy regeneration after the adsorption reaches a saturated state, no corrosivity to an adsorption device and the like. Is widely applied to the fields of food industry, chemical industry, environmental protection and the like. Since the beginning of the last century, activated carbon has been used as a typical adsorbent in wastewater and exhaust gas treatment processes. Traditional commercial activated carbon generally takes minerals as raw materials, especially coal-based activated carbon, and is widely applied in production. But coal mine resources are not renewable.
In the prior art, the activated carbon material comprises a biological material, a composite material and the like, wherein the plant-based activated carbon is considered to be the most potential choice for treating water environment pollution due to the advantages of low price, easy obtainment, environmental protection and economy. The plant material is the material with the most abundant sources and the largest yield on the earth, and can be recycled, so the plant material has good development prospect.
The plant-based activated carbon has a large specific surface area and rich pore structures, so the plant-based activated carbon has a good adsorption effect and has great potential in removing pollutants in a water environment.
Disclosure of Invention
The invention aims to solve the technical problem of providing plant-based activated carbon and a preparation method and application thereof.
The invention also provides a preparation method of the plant-based activated carbon, which comprises the step of carbonizing plant raw materials in a protective gas atmosphere to obtain the plant-based activated carbon.
Preferably, the plant raw material is pretreated, wherein the pretreatment comprises the steps of soaking the plant raw material in absolute ethyl alcohol for 0.5-2 hours, cleaning with deionized water, and drying at 55-65 ℃ for 1-3 hours.
The plant material is any one of miscanthus, guar gum and lotus seedpod.
Preferably, the protective gas is at least one of argon, nitrogen or helium, preferably nitrogen.
Preferably, the purity of the protective gas is 95% to 99.9%, preferably 99.9%.
Preferably, the carbonization conditions are: heating to 300-800 ℃ at a speed of 1-8 ℃/min, and preserving heat for 1-2 h.
More preferably, the carbonization conditions are: heating to 700-800 ℃ at a speed of 2-3 ℃/min, and preserving heat for 1-2 h.
Further preferably, the carbonization conditions are as follows: heating to 800 deg.C at a speed of 2 deg.C/min, and maintaining for 2 hr.
The invention provides plant-based activated carbon prepared by any one of the methods.
The microstructure of the plant-based activated carbon is long tubular, and the inside of the pipeline is provided with a rich pore structure.
Preferably, the aperture of the plant-based activated carbon is 2-10 μm, and the porosity is 70% -80%.
More preferably, the plant-based activated carbon has a pore diameter of 4 μm and a porosity of 75%.
The invention also provides application of the plant-based activated carbon in adsorbing antibiotic pollutants.
The invention also provides an adsorbent for adsorbing antibiotic pollutants, which comprises the plant-based activated carbon prepared by any one of the methods.
The invention also provides a method for adsorbing antibiotic pollutants by using the plant-based activated carbon, which comprises the steps of adding the plant-based activated carbon into liquid containing antibiotics and stirring.
The invention also provides a method for testing the adsorption capacity of the plant-based activated carbon for adsorbing the antibiotic pollutants, which comprises the steps of preparing a series of antibiotic solutions with concentration gradients, adding the plant-based activated carbon for adsorbing the antibiotic pollutants, stirring for 4-12 hours, measuring absorbance under characteristic wavelength by using an ultraviolet spectrophotometer, calculating the solution concentration according to the absorbance, and further calculating to obtain the adsorption capacity.
The concentration of the antibiotic solution is 10-100 mg/L, and the volume of the antibiotic solution is 80-120 mL.
Preferably, the concentration of the antibiotic solution is 10-40mg/L, and the volume is 95-105 mL.
The characteristic wavelength is 260-280nm, and the preferred wavelength is 277 nm.
The dosage of the added plant-based activated carbon is 0.1-1 mg, preferably 0.1-0.2 mg.
The stirring speed is 500-1000 rpm, preferably 600-700 rpm.
The antibiotic is quinoline antibiotic.
The antibiotic solution is prepared by adopting the following method: weighing quinoline antibiotics, fully dissolving the quinoline antibiotics in deionized water, then fixing the volume by using a 500mL volumetric flask to prepare quinoline antibiotic solution with the initial concentration of 40mg/L, and then preparing antibiotic solution with 10-40mg/L series concentration gradient by using a 100mL conical flask.
According to the method, common plants are used as raw materials, under the atmosphere of protective gas, through regulating and controlling experimental parameters such as heating temperature, heating rate, heat preservation time and the like, carbonization is further completed, the particle size of the plant-based activated carbon is refined, and the bio-based activated carbon material with a unique structure, a large specific surface area and excellent adsorption performance is prepared, and the adsorption of the bio-based activated carbon material can reach 400-600 mg/g.
Compared with the prior art, the invention has the following advantages:
(1) the plant-based active carbon material selected by the invention is a common plant in the nature, has wide distribution field and can be prepared in a large scale.
(2) The plant-based activated carbon material prepared by the method has the advantages of large specific surface area, abundant pore channel structures on the surface, good antibiotic adsorption performance, and especially excellent antibiotic adsorption performance with ultralow concentration.
(3) The preparation method is simple, does not need complex equipment, does not involve the use of expensive reactants, and has low cost.
(4) The plant-based activated carbon prepared by the invention is used for adsorption, and can expand the preparation method and application field of the adsorption material.
Drawings
FIG. 1 is a scanning electron microscope image of a plant-based activated carbon material prepared from miscanthus sinensis.
FIG. 2 is a high power scanning electron microscope picture of a plant-based activated carbon material prepared from miscanthus sinensis.
Detailed Description
Example 1
A preparation method of plant-based activated carbon comprises the following steps: soaking guar gum in absolute ethyl alcohol for 1h, then washing with deionized water, taking out, drying in a forced air drying oven at the temperature of 60 ℃ for 2h, transferring to a tubular furnace, introducing nitrogen, heating to 800 ℃ at the heating rate of 2 ℃/min, preserving heat for 2h, carbonizing, and cooling to obtain the plant-based activated carbon.
The obtained plant-based activated carbon has the pore diameter of 2-50 nm, the pore diameter is mostly distributed at 4nm, the porosity is 70% -80%, and the porosity is mostly distributed at 75%.
The method for testing the adsorption capacity of the plant-based activated carbon for adsorbing the antibiotic pollutants comprises the following steps: weighing 20mg of quinoline antibiotic, fully dissolving in 200mL of deionized water, and then adding a 500mL volumetric flask to a constant volume to prepare a quinoline antibiotic solution with the initial concentration of 40 mg/L. Then diluting the initial solution to prepare a 5-40mg/L antibiotic solution with the volume of 100 mL. Adding 0.1mg of plant-based activated carbon into the antibiotic solution with the concentration of 5mg·L-1，10mg·L-1，15mg·L-1，20mg·L-1，25mg·L-1，30mg·L-1，35mg·L-1，40mg·L-1The antibiotic solution is stirred for 6 hours at the rotating speed of 600r/min to adsorb antibiotic pollutants. Measuring absorbance at characteristic wavelength with ultraviolet spectrophotometer, fitting Langmuir formula after obtaining original data, and fitting antibiotic (quinoline) adsorption result below 10ppm to 425mg g-1。
Example 2
The preparation method of the plant-based activated carbon comprises the following steps: removing branches and stems of miscanthus sinensis, soaking the flocculent head part in absolute ethyl alcohol for 1h, then cleaning with deionized water, taking out, drying in a blast drying oven at the temperature of 60 ℃ for 2h, transferring to a tubular furnace, introducing nitrogen, raising the temperature to 750 ℃ at the temperature raising rate of 2.5 ℃/min, preserving the temperature for 1.5h for carbonization, and cooling to obtain the plant-based activated carbon, wherein SEM pictures are shown in figures 1 and 2.
The obtained plant-based activated carbon has the pore diameter of 2-50 nm, the pore diameter is mostly distributed at 4nm, the porosity is 70% -80%, and the porosity is mostly distributed at 75%.
The method for testing the adsorption capacity of the plant-based activated carbon for adsorbing the antibiotic pollutants comprises the following steps: weighing 20mg of quinoline antibiotic, fully dissolving in 200mL of deionized water, and then adding a 500mL volumetric flask to a constant volume to prepare a quinoline antibiotic solution with the initial concentration of 40 mg/L. Then diluting the initial solution to prepare a 5-40mg/L antibiotic solution with the volume of 100 mL. Adding 0.15mg of plant-based activated carbon into the antibiotic solution with the concentration of 5 mg.L-1，10mg·L-1，15mg·L-1，20mg·L-1，25mg·L-1，30mg·L-1，35mg·L-1，40mg·L-1The antibiotic solution is stirred for 6 hours at the rotating speed of 600r/min to adsorb antibiotic pollutants. Measuring absorbance at characteristic wavelength with ultraviolet spectrophotometer, fitting Langmuir formula after obtaining original data, and fitting antibiotic (quinoline) adsorption result to 290mg g-1。
Example 3
The preparation method of the plant-based activated carbon comprises the following steps: removing lotus seeds from lotus seedpods, soaking the lotus seedpods in absolute ethyl alcohol for 1h, then cleaning the lotus seedpods with deionized water, taking the lotus seedpods out, drying the lotus seedpods in a blast drying oven at the temperature of 60 ℃ for 2h, transferring the lotus seedpods to a tubular furnace, introducing nitrogen, heating the lotus seedpods to 700 ℃ at the heating rate of 3 ℃/min, preserving the temperature for 1h, carbonizing the lotus seedpods, and cooling the lotus seedpods to obtain the plant-based activated carbon.
The aperture of the obtained activated carbon structure is 2-10 mu m, and the aperture is mostly distributed in 4 mu m; the porosity is 70-80%, and the porosity is mostly distributed at 75%.
The method for testing the adsorption capacity of the plant-based activated carbon for adsorbing the antibiotic pollutants comprises the following steps: weighing 20mg of quinoline antibiotic, fully dissolving in 200mL of deionized water, and then adding a 500mL volumetric flask to a constant volume to prepare a quinoline antibiotic solution with the initial concentration of 40 mg/L. Then diluting the initial solution to prepare a 5-40mg/L antibiotic solution with the volume of 100 mL. Adding 0.2mg of plant-based activated carbon into the antibiotic solution with the concentration of 5 mg.L-1，10mg·L-1，15mg·L-1，20mg·L-1，25mg·L-1，30mg·L-1，35mg·L-1，40mg·L-1The antibiotic solution is stirred for 6 hours at the rotating speed of 600r/min to adsorb antibiotic pollutants. Measuring absorbance at characteristic wavelength with ultraviolet spectrophotometer, obtaining original data, fitting Langmuir formula, and fitting antibiotic (quinoline) adsorption result to 100mg g-1。
The above embodiments are described to facilitate understanding and use by those of ordinary skill in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art can make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The preparation method of the plant-based activated carbon is characterized by comprising the step of carbonizing a plant raw material in a protective gas atmosphere to obtain the plant-based activated carbon.
2. The method for preparing a plant-based activated carbon as claimed in claim 1, wherein the plant material is pretreated by immersing the plant material in absolute ethanol for 0.5 to 2 hours, washing with deionized water, and drying at 55 to 65 ℃ for 1 to 3 hours.
3. The method of making a plant-based activated carbon as in claim 1, wherein the plant material is any one of miscanthus, guar gum, lotus seedpod.
4. The method of making plant-based activated carbon as claimed in claim 1, wherein the carbonization conditions are: heating to 300-800 ℃ at a speed of 1-8 ℃/min, and preserving heat for 1-2 h.
5. The method of making plant-based activated carbon as claimed in claim 1, wherein the carbonization conditions are: heating to 700-800 ℃ at a speed of 2-3 ℃/min, and preserving heat for 1-2 h.
6. A plant-based activated carbon produced by the method for producing a plant-based activated carbon according to any one of claims 1 to 5.
7. The plant-based activated carbon as claimed in claim 6, which is characterized in that: the microstructure is long tubular, the aperture is 2-10 μm, and the porosity is 70% -80%.
8. Use of a plant-based activated carbon as claimed in claim 6 or claim 7 for the adsorption of antibiotic contaminants.
9. An adsorbent for adsorption of antibiotic contaminants, comprising the plant-based activated carbon of claim 6 or 7.
10. A method for adsorbing antibiotic contaminants on plant-based activated carbon, comprising adding the plant-based activated carbon according to claim 6 or 7 to a liquid containing an antibiotic, and stirring.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113289576A (en) * | 2021-04-29 | 2021-08-24 | 长江大学 | Lotus seedpod hydrothermal carbon and preparation method and application thereof |
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2019
- 2019-11-22 CN CN201911157963.1A patent/CN110817864A/en active Pending
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| EP2308591A1 (en) * | 2008-07-31 | 2011-04-13 | Sony Corporation | Adsorbent, cleansing agent, remedy for kidney disease and functional food |
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| CN113289576A (en) * | 2021-04-29 | 2021-08-24 | 长江大学 | Lotus seedpod hydrothermal carbon and preparation method and application thereof |
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Application publication date: 20200221 |