CN107715836B - Preparation method of iron-based porous carbon composite adsorption material based on biomass - Google Patents
Preparation method of iron-based porous carbon composite adsorption material based on biomass Download PDFInfo
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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
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/10—Inorganic compounds
Abstract
The invention relates to a preparation method of a biomass-based iron-based porous carbon composite adsorption material, which takes palm filaments as raw materials and comprises the following steps: firstly, washing palm filaments, drying at 50-80 ℃ and cutting; secondly, putting the palm fibers into a sodium hydroxide solution, stirring, filtering, washing until the pH value is neutral, and drying; and thirdly, pre-oxidizing the palm fibers at the temperature of 200-400 ℃ in the air atmosphere for 1-5 hours, cooling to room temperature, then heating to 600-1200 ℃ at the heating rate of 1-5 ℃/min under the protection of nitrogen, keeping the temperature for 60-240 minutes, finally controlling the cooling rate to be 2-10 ℃/min, cooling to room temperature, taking out, soaking in an iron salt solution, filtering after soaking, heating to 800 ℃ at the heating rate of 1-5 ℃/min under the protection of nitrogen again, keeping the temperature for 30-240 minutes, and finally controlling the cooling rate to be 2-10 ℃/min, cooling to room temperature, thus obtaining the composite adsorbing material. The adsorbing material prepared by the invention has a removal rate of more than 95% in a wider pH value range for molybdate ions.
Description
Technical Field
The invention relates to the technical field of heavy metal ion adsorption materials, and particularly relates to a preparation method of a biomass-based porous carbon composite adsorption material.
Background
In recent years, as the production and living level of people is continuously improved, the circulation of heavy metals in the natural world is continuously increased, the original biological geochemical balance is destroyed, the content of the heavy metals in local areas or regions exceeds the environmental capacity, the water quality of rivers and lakes is rapidly reduced due to the pollution of industrial waste water and urban domestic sewage and the heavy metal pollution of mines and metallurgical industry, the water quality is seriously influenced, even the health of people is harmed, the heavy metals in the polluted water mainly comprise Mo, Hg, Cd, Pb, Cr, Zn, Cu, Co and the like, wherein the heavy metals are not only one of nutrient elements necessary for the growth of animals and plants, but also very important strategic resources, and the molybdenum in the environment has two sources, namely ① weathering effect enables the molybdenum to be released from rocksThe molybdenum is more and more widely applied to the human activities of ② and the molybdenum is burnt with molybdenum-containing mineral fuel (such as coal) so as to increase the circulation amount of the molybdenum in the environment, the average abundance of the molybdenum in the earth crust is 1.3ppm, the molybdenum is mostly present in molybdenite, molybdenite and hydromolybdenite, and when the interior of molybdenum tailings presents an acidic or alkaline environment, such as molybdenite (MoS)2) All can be converted into MoO4 2-. The maximum allowable concentration of molybdenum in ground water is 0.5 mg/L, however, the molybdenum mining technology is relatively laggard in China, and the tailings management is insufficient, so that relatively serious molybdenum pollution events are generated in some areas, such as the molybdenum mine areas in Luoyang goldthread and the molybdenum mine areas in Fenugui city in Liaoning province. At present, research work on heavy metal molybdenum mainly focuses on the influence and harm of molybdenum deficiency on animals and plants, and research on environmental problems caused by molybdenum pollution and solution is rare, so that the research on treatment of heavy metal molybdenum pollution is necessary. In 2005, in the city of the Fenugu island in Liaoning province, due to molybdenum pollution of the reservoir water source place of the Ujin pond, water sources must be found in the whole city, and although the molybdenum sewage in the reservoir is treated by adopting a chemical process method at present so that the molybdenum sewage can supply water, the molybdenum sewage can not meet the requirements of local residents, and the molybdenum pollution of the warehousing river can not be prevented and controlled by the method. The over-accumulation of the molybdenum tailings in the Luoyang goldenrain causes pollution to local water sources to different degrees, so that a great amount of fishes die, and the local living environment is also influenced.
At present, the treatment technology (including artificial wetland method, chemical precipitation method, ion exchange method and adsorption method) for molybdenum pollution in the environment at home and abroad. Although the constructed wetland can separate molybdenum from a water body, the matrix containing molybdenum and functional plants have uncontrollable risks such as pollution transfer and the like; the chemical precipitation method has good effect of removing medium-low concentration sewage, but the excess sludge is difficult to treat and can not be recycled; the ion exchange method can effectively separate the polluted molybdenum from the water body, and realizes the repeated utilization of the resin through desorption, but the resin has poor adaptability and higher requirements on reaction control conditions such as pH value and the like; the traditional adsorption method mainly using materials uses cheap materials to enrich pollutants, but has the problem of secondary pollution. Therefore, by combining the advantages and the disadvantages of different adsorbing materials, the preparation of the biomass composite material and the application of the biomass composite material as the adsorbing material of heavy metal ions in wastewater have great research value and application prospect.
Disclosure of Invention
The invention aims to solve the technical problems and provide a preparation method of an iron-based porous carbon composite adsorbing material based on biomass, wherein palm fibers are used as raw materials, and the prepared adsorbing material has a removal rate of more than 95% on molybdate ions within a wider pH value range.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a biomass-based iron-based porous carbon composite adsorption material comprises the following steps:
firstly, washing palm filaments, drying at 50-80 ℃, and chopping for later use;
secondly, putting the palm fibers into a sodium hydroxide solution, stirring, filtering, washing until the pH value is neutral, and drying for later use;
and thirdly, pre-oxidizing the palm fibers at the temperature of 200-400 ℃ in the air atmosphere for 1-5 hours, cooling to room temperature, then heating to 600-1200 ℃ at the heating rate of 1-5 ℃/min under the protection of nitrogen, keeping the temperature for 60-240 minutes, finally controlling the cooling rate to be 2-10 ℃/min, cooling to room temperature, taking out, soaking in an iron salt solution, filtering after soaking, heating to 800 ℃ at the heating rate of 1-5 ℃/min under the protection of nitrogen again, keeping the temperature for 30-240 minutes, and finally cooling to room temperature at the cooling rate of 2-10 ℃/min to obtain the iron-based porous carbon composite adsorbing material.
The preparation method based on the biomass iron-based porous carbon composite adsorption material is further optimized as follows: the first step is specifically as follows: washing palm silk with water at room temperature for several times until no dust and other impurities are attached to the surface, drying at 50-80 deg.C, and cutting into 0.1-2 cm.
The preparation method based on the biomass iron-based porous carbon composite adsorption material is further optimized as follows: the second step is specifically as follows: the palm silk is put into sodium hydroxide solution with the concentration of 2-5mol/L and stirred for 30-180 minutes at the temperature of 60-120 ℃.
The preparation method based on the biomass iron-based porous carbon composite adsorption material is further optimized as follows: the concentration of the ferric salt solution in the third step is 0.5-3 mol/L.
The preparation method based on the biomass iron-based porous carbon composite adsorption material is further optimized as follows: the ferric salt in the ferric salt solution is FeCl3·6H2O、Fe(NO3)3·9H2O、FeSO4·7H2O and Fe2(SO4)3·9H2One or any mixture of O.
Advantageous effects
The adsorbing material prepared by the invention can adsorb molybdate ions in wastewater and polluted water, has a large pH range, a large adsorption capacity, no pollution and can be recycled, and according to adsorption test data, the adsorbing material disclosed by the invention has a removal rate of more than 95% for the molybdate ions within a wider pH value range;
the biomass iron-based porous carbon composite adsorption material is prepared by taking the palm fibers as raw materials, the method is simple, the process is controllable, the raw material source is rich, and the prepared adsorption material has stable adsorbent performance and can be stored and used for a long time.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments.
Example 1
A preparation method of an iron-based porous carbon composite adsorption material based on biomass comprises the following steps:
firstly, cutting palm fiber from palm, washing 100 g of palm fiber with water at room temperature for 5 times until no dust and other impurities are attached to the surface, drying at 60 ℃, and cutting into 0.5 cm for later use.
Secondly, placing the short palm fibers in a sodium hydroxide solution with the concentration of 2mol/L, stirring for 60 minutes at the temperature of 80 ℃, filtering, washing until the pH value is about 7, and drying for later use.
Thirdly, pre-oxidizing the palm fibers treated by the alkali in the air atmosphere at the temperature of 300 ℃ for 2 hours, and cooling to room temperature; and then under the protection of nitrogen, heating to 700 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 180 minutes at a cooling rate of 10 ℃/min, and taking out until the temperature is room temperature to obtain the porous carbon material. And (2) soaking the porous carbon material in a ferric chloride solution with the concentration of 1mol/L for 120 minutes, filtering, washing away ferric chloride on the surface, heating to 600 ℃ at the heating rate of 2 ℃/min under the protection of nitrogen again, keeping the temperature for 60 minutes at the constant temperature, and taking out at the cooling rate of 10 ℃/min until the temperature is room temperature, thereby obtaining the iron-based porous carbon composite material.
By adjusting 100 parts of raw water and the pH value to 3.0, 3 parts of the iron-based porous carbon composite material is added, the stirring time is 60 minutes, and the removal rate of molybdenum in sewage is up to more than 98%.
Example 2:
a preparation method of an iron-based porous carbon composite adsorption material based on biomass comprises the following steps:
firstly, cutting palm fiber from palm, washing 50 g of palm fiber with water at room temperature for 3 times until no dust and other impurities are attached to the surface, drying at 50 ℃, and cutting into 1 cm for later use.
Secondly, placing the short palm fibers in a sodium hydroxide solution with the concentration of 1mol/L, stirring for 120 minutes at the temperature of 120 ℃, filtering, washing until the pH value is about 7, and drying for later use.
Thirdly, pre-oxidizing the palm fibers treated by the alkali in the air atmosphere at the temperature of 400 ℃ for 2 hours, and cooling to room temperature; and then under the protection of nitrogen, heating to 800 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 120 minutes at the cooling rate of 10 ℃/min, and taking out until the temperature is room temperature to obtain the porous carbon material. Soaking the porous carbon material in a solution containing ferric chloride and ferric sulfate with the concentration of 0.5mol/L for 90 minutes, filtering, washing away the ferric chloride and ferric sulfate on the surface, heating to 500 ℃ at the heating rate of 2 ℃/min under the protection of nitrogen again, keeping the temperature for 120 minutes at the constant temperature at the cooling rate of 10 ℃/min, and taking out until the temperature reaches room temperature to obtain the iron-based porous carbon composite material.
By adjusting 50 parts of raw water and the pH value to 4.0, 2 parts of the iron-based porous carbon composite material is added, the stirring time is 120 minutes, and the removal rate of molybdenum in sewage is up to more than 97%.
Example 3:
a preparation method of an iron-based porous carbon composite adsorption material based on biomass comprises the following steps:
firstly, cutting palm fiber from palm, washing 200 g of palm fiber with water at room temperature for 4 times until no dust and other impurities are attached to the surface, drying at 80 ℃, and cutting into 1.5 cm for later use.
Secondly, placing the short palm fibers in a sodium hydroxide solution with the concentration of 5mol/L, stirring for 90 minutes at the temperature of 60 ℃, filtering, washing until the pH value is about 7, and drying for later use.
Thirdly, pre-oxidizing the palm fibers treated by the alkali in the air atmosphere at the temperature of 200 ℃ for 4 hours, and cooling to room temperature; and then under the protection of nitrogen, heating to 800 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 60 minutes at the constant temperature, and taking out at the cooling rate of 10 ℃/min until the temperature is room temperature, thus obtaining the porous carbon material. Soaking the porous carbon material in a ferric sulfate solution with the concentration of 3mol/L for 100 minutes, filtering, washing away ferric sulfate on the surface, heating to 700 ℃ at the heating rate of 2 ℃/min again under the protection of nitrogen, keeping the temperature for 120 minutes at the constant temperature, and taking out at the cooling rate of 5 ℃/min until the temperature is room temperature, thus obtaining the iron-based porous carbon composite material.
By adjusting 200 parts of raw water and 3.0 of pH value, 5 parts of the iron-based porous carbon composite material is added, the stirring time is 80 minutes, and the removal rate of molybdenum in sewage is up to more than 97%.
Example 4:
a preparation method of an iron-based porous carbon composite adsorption material based on biomass comprises the following steps:
firstly, cutting palm fiber from palm, washing 100 g of palm fiber with water at room temperature for 4 times until no dust and other impurities are attached to the surface, drying at 80 ℃, and cutting into 2 cm for later use.
Secondly, placing the short palm fibers in a sodium hydroxide solution with the concentration of 5mol/L, stirring for 90 minutes at the temperature of 100 ℃, filtering, washing until the pH value is about 7, and drying for later use.
Thirdly, pre-oxidizing the palm fibers treated by the alkali in the air atmosphere at the temperature of 250 ℃ for 5 hours, and cooling to room temperature; and then under the protection of nitrogen, heating to 1000 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 90 minutes at a cooling rate of 10 ℃/min, and taking out until the temperature is room temperature to obtain the porous carbon material. And (2) soaking the porous carbon material in a ferric nitrate solution with the concentration of 2mol/L for 60 minutes, filtering, washing away ferric nitrate on the surface, heating to 650 ℃ again under the protection of nitrogen at the heating rate of 2 ℃/min, keeping the temperature for 240 minutes at the constant temperature, and taking out at the cooling rate of 10 ℃/min until the temperature is room temperature, thereby obtaining the iron-based porous carbon composite material.
By adjusting 100 parts of raw water and the pH value to 6.0, 4 parts of the iron-based porous carbon composite material is added, the stirring time is 100 minutes, and the removal rate of molybdenum in sewage is up to more than 96%. And taking out the used adsorbent through a magnet, further under the protection of nitrogen, heating to 600 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 180 minutes at a constant temperature, and cooling at a cooling rate of 10 ℃/min until the temperature is room temperature, and taking out the adsorbent until the temperature is room temperature to obtain the iron-based porous carbon composite material, and adsorbing molybdate ions in the wastewater again, wherein the removal rate is more than 96%.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. A preparation method of a biomass-based iron-based porous carbon composite adsorption material is characterized by comprising the following steps: the method comprises the following steps:
firstly, washing palm filaments, drying at 50-80 ℃, and chopping for later use;
secondly, putting the palm fibers into a sodium hydroxide solution with the concentration of 2-5mol/L, stirring for 30-180 minutes at the temperature of 60-120 ℃, filtering, washing until the pH value is neutral, and drying for later use;
and thirdly, pre-oxidizing the palm fibers treated in the second step for 1-5 hours at the temperature of 200-400 ℃ in the air atmosphere, cooling to room temperature, then heating to 600-1200 ℃ at the heating rate of 1-5 ℃/min under the protection of nitrogen, keeping the temperature for 60-240 minutes, finally controlling the cooling rate to 2-10 ℃/min, cooling to room temperature, taking out, soaking in an iron salt solution, filtering after soaking, heating to 800 ℃ at the heating rate of 1-5 ℃/min under the protection of nitrogen again, keeping the temperature for 30-240 minutes, finally controlling the cooling rate to 2-10 ℃/min, cooling to room temperature, and obtaining the iron-based porous carbon composite adsorbing material.
2. The preparation method of the biomass-based iron-based porous carbon composite adsorption material according to claim 1, characterized by comprising the following steps: the first step is specifically as follows: washing palm silk with water at room temperature for several times until no dust and other impurities are attached to the surface, drying at 50-80 deg.C, and cutting into 0.1-2 cm.
3. The preparation method of the biomass-based iron-based porous carbon composite adsorption material according to claim 1, characterized by comprising the following steps: the concentration of the ferric salt solution in the third step is 0.5-3 mol/L.
4. The preparation method of the biomass-based iron-based porous carbon composite adsorption material according to claim 3, characterized by comprising the following steps: the ferric salt in the ferric salt solution is FeCl3·6H2O、Fe(NO3)3·9H2O、FeSO4·7H2O and Fe2(SO4)3·9H2One or any mixture of O.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2786499C1 (en) * | 2022-11-10 | 2022-12-21 | федеральное государственное бюджетное образовательное учреждение высшего образования "Донской государственный технический университет" (ДГТУ) | Method for obtaining an adsorbent from palm leaves for water treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108993408B (en) * | 2018-07-13 | 2021-04-09 | 南京波顿夫哲材料科技有限公司 | Preparation method of porous adsorption-catalysis material for waste gas treatment based on biomass |
| CN108987733B (en) * | 2018-09-11 | 2021-04-27 | 郑州大学 | Preparation method of active porous carbon @ FeS of lithium ion battery cathode material |
| CN113430565B (en) * | 2021-06-16 | 2022-10-11 | 江西师范大学 | Method for preparing carbon-based transition metal nano composite catalyst from tremella |
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| CN104692381A (en) * | 2015-03-04 | 2015-06-10 | 河南工程学院 | Preparation method of superhigh-specific-area activated carbon fibers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2786499C1 (en) * | 2022-11-10 | 2022-12-21 | федеральное государственное бюджетное образовательное учреждение высшего образования "Донской государственный технический университет" (ДГТУ) | Method for obtaining an adsorbent from palm leaves for water treatment |
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Effective date of registration: 20230407 Address after: 2nd Floor, Hongchu Technology Building, No. 18 Chuncheng Road, High tech Zone, Luoyang Area, China (Henan) Free Trade Pilot Zone, Luoyang City, Henan Province, 471000 Patentee after: LUOYANG BAKU BIO-TECH Co.,Ltd. Address before: No.71, Luolong Road, Luolong District, Luoyang City, Henan Province Patentee before: LUOYANG NORMAL University |