WO2024251202A1 - Méthode de préparation d'un matériau carboné poreux au moyen d'une modification de boue rouge et utilisation d'un matériau carboné poreux - Google Patents

Méthode de préparation d'un matériau carboné poreux au moyen d'une modification de boue rouge et utilisation d'un matériau carboné poreux Download PDF

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WO2024251202A1
WO2024251202A1 PCT/CN2024/097780 CN2024097780W WO2024251202A1 WO 2024251202 A1 WO2024251202 A1 WO 2024251202A1 CN 2024097780 W CN2024097780 W CN 2024097780W WO 2024251202 A1 WO2024251202 A1 WO 2024251202A1
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red mud
carbon material
porous carbon
fluorine
adsorption
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Chinese (zh)
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李彬
张利平
王建城
曾和平
钱文敏
杨花
彭庆收
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Binzhou Weiqiao National Science And Technology Advanced Technology Research Institute
Kunming University of Science and Technology
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Binzhou Weiqiao National Science And Technology Advanced Technology Research Institute
Kunming University of Science and Technology
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • 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

Definitions

  • the present application belongs to the technical field of solid waste resource utilization, and specifically relates to a method for preparing porous carbon materials by modifying red mud and its application.
  • Red mud is a major solid waste generated during the production of alumina. Depending on the quality of alumina and the production process, red mud can be divided into Bayer red mud , sintering red mud and combined red mud. Red mud contains a large amount of metal oxides such as Fe2O3 , Al2O3 and TiO2 , and has the potential to become an effective material for treating atmospheric pollutants.
  • the traditional method of treating red mud is mainly stockpiling, which not only occupies land resources, but also the heavy metals in the red mud will penetrate into the ground through surface water and rainwater leaching, polluting the surrounding soil and causing soil salinization. At the same time, small particles on the surface of red mud will also diffuse into the air, causing air pollution. Therefore, improving its comprehensive utilization rate is the key to solving the problem of large-scale accumulation of red mud.
  • plastic As an organic polymer material, plastic is widely used in industrial production and daily life because of its convenience, low cost, lightness, high strength and corrosion resistance. However, plastic is prone to aging and damage during use, has a short service life, and is difficult to degrade in the natural environment. If untreated waste plastic is directly discharged into the environment, it will cause white pollution and trigger a serious ecological crisis.
  • the main methods for treating plastics include landfill, incineration and pyrolysis. Although landfill is the simplest method, it requires a lot of land resources; and the incineration process will produce a large amount of harmful gases, which will cause secondary pollution if leaked into the air.
  • the emission reduction technologies for PFCs are mainly combustion, cracking, catalysis and adsorption.
  • adsorption is considered to be a promising technology for capturing PFCs due to its low energy consumption, low cost and easy management.
  • porous carbon materials are widely used due to their low preparation cost, large specific surface area, developed pore structure, good chemical and mechanical stability, and relatively easy regeneration.
  • a certain amount of pore structure can be obtained by treating carbon materials with physical or chemical activation methods, physical activation requires very high temperatures and a long time, and the increase in the specific surface area of the activated carbon materials is relatively limited.
  • the carbon materials after chemical activation need to be cleaned to remove the activator residues in the pores, which further increases the cost of the reaction.
  • the treatment of red mud and waste plastics in China in terms of adsorbents mainly focuses on using acid and alkali to treat red mud or activating agents to treat waste plastics to prepare adsorbents.
  • the materials prepared in this way cannot fully utilize the metal oxides, specific surface area and pore structure contained therein, making it difficult to achieve efficient adsorption and purification performance, and it is difficult to achieve the goal of solid waste resource utilization.
  • the present application provides a method for preparing porous carbon materials by combining red mud with plastic modification and for adsorbing and treating fluorine-containing gases.
  • the method adopts a catalytic activation method, utilizes the abundant metal oxides such as Fe2O3 in red mud to dope with carbon materials, and then activates them to increase the surface active points of the micropores inside the carbon materials, so that the micropores are transformed into mesopores, thereby improving the adsorption effect of the porous carbon adsorbent and achieving the effect of purifying the fume of electrolytic aluminum.
  • the present application uses red mud and waste plastic bottles as raw materials, and through simple carbonization and activation, the prepared porous carbon adsorbent has better adsorption properties, which can not only remove PFCs in the flue gas of electrolytic aluminum, but also reduce the pollution of red mud to the environment and realize the resource utilization of red mud. At the same time, it realizes the environmentally friendly utilization of waste within the aluminum industry, reduces the cost of environmental governance, and achieves the purpose of synergistic efficiency improvement of pollution reduction and carbon reduction.
  • a method for preparing porous carbon material by modifying red mud the specific steps are as follows:
  • the citric acid in the citric acid solution in step (1) accounts for 1-10% of the mass of the red mud powder.
  • the main component of the waste plastic bottles in step (2) is polyethylene (PE).
  • the carbonization in step (2) is: heating to 450-600°C at a heating rate of 5°C/min and calcining for 3h under N2 atmosphere.
  • the mass ratio of the carbon material to the red mud powder is 1:2-4.
  • the rotation speed of the magnetic stirring in step (1) and step (2) is independently 300-500 rpm; and the equipment for magnetic stirring is a magnetic stirrer.
  • the vacuum drying temperature in step (3) is 60-80° C., and the vacuum drying time is 12 h.
  • the calcination activation in step (3) is: heating to 500-800°C at a heating rate of 5°C/min under N2 atmosphere and calcining for 3h.
  • the present application also provides an application of the red mud-based porous carbon material prepared by the method described in the above technical scheme for adsorbing and treating fluorine-containing gases, and the application is: placing the red mud-based porous carbon material in a fixed bed reactor, pretreating it at 300°C for 2h under a N2 atmosphere, passing fluorine-containing gas after cooling to 120°C, and performing adsorption purification. After the red mud-based porous carbon material is saturated with adsorption, heating it to 150°C for desorption, collecting the desorbed gas, and using the red mud-based porous carbon material again as an adsorption material after desorption to adsorb and purify the fluorine-containing gas.
  • the fluorine-containing gas includes 2% C 2 F 6 , 2% CF 4 , 2% CO 2 , and 94% N 2 .
  • the flow rate of the fluorine-containing gas is 200 mL/min.
  • the desorption is N2 purging desorption; and the desorption time is 3h.
  • the adsorption amount of perfluorocarbon by the red mud-based porous carbon material is 1.75 mmol/g, 2.15 mmol/g, 2.45 mmol/g, 2.48 mmol/g, 2.34 mmol/g, 2.54 mmol/g or 1.90 mmol/g.
  • the fluorine-containing gas is aluminum electrolysis fume.
  • the present application uses red mud loaded carbonized plastic to prepare porous carbon materials for adsorbing and treating PFCs in electrolytic aluminum flue gas. Compared with adsorption materials prepared using red mud or waste plastic alone, this has better effects, not only improving the PFCs removal rate, but also reducing the generation of HF and CO2 gases, thus providing a new method for the resource utilization of red mud.
  • porous carbon material prepared in the present application adsorbs PFCs
  • high-concentration PFCs can be obtained through adsorption-desorption, which can reduce the energy consumption of subsequent treatments such as plasma decomposition and thermal catalysis.
  • This application converts waste plastic bottles into carbon materials as carriers, and then loads the metal oxides in red mud It increases the surface area of the material and the selectivity of the gas, alleviating the impact of waste plastics on the environment.
  • the present application utilizes the method of “treating waste with waste”, which not only improves the utilization rate of red mud and plastics, but also reduces process costs and reduces pollution to the environment.
  • FIG1 is a process flow chart of red mud modification to prepare porous carbon materials for treating fluorine-containing gases.
  • the red mud used in the examples of the present application comes from an aluminum company in Wenshan City, Yunnan province.
  • a method for preparing porous carbon materials by modifying red mud and its application in adsorbing and treating fluorine-containing gases, as shown in FIG1 has the following specific steps:
  • Red mud from an aluminum company in Wenshan City, Yunnan province was placed in an oven at 100°C and dried to constant weight, and then ground to pass through a 100-mesh sieve to obtain red mud powder for use; then an appropriate amount of the red mud powder was taken into a beaker, and a citric acid solution was added for acid treatment, wherein the citric acid in the citric acid solution accounted for 1% of the mass of the red mud powder to remove alkali metals and adhesive components in the red mud, and the red mud was placed in a magnetic stirrer and stirred at room temperature for 20 minutes at a speed of 300 rpm, and then filtered and washed with deionized water until the pH was neutral to obtain a red mud slurry for use;
  • step (3) The carbon material obtained in step (2) is added to the red mud slurry in a mass ratio of 1:2 with the red mud powder obtained in step (1) and mixed.
  • the mixture is placed in a magnetic stirrer and stirred at room temperature for 2 h at a rotation speed of 300 rpm.
  • the formed mixture is placed in a vacuum drying oven at 60°C for 12 h to remove moisture.
  • the dried mixture is then placed in a tubular furnace under a N2 atmosphere and heated to 500°C at a heating rate of 5°C/min and calcined for 3 h. After the calcination temperature is cooled to room temperature, a red mud-based porous carbon material is obtained.
  • the red mud-based porous carbon material was placed in a fixed bed reactor and pretreated at 300°C for 2 h under N 2 atmosphere. After cooling to 120°C, a fluorine-containing mixed gas (2% C 2 F 6 , 2% CF 4 , 2% CO 2 , 94% N 2 ) was introduced at a gas flow rate of 200 mL/min. The outlet gas was tested for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, adsorption saturation was achieved. Then the fixed bed reactor was placed in a fixed bed reactor and the adsorption was carried out. The temperature of the reactor was raised to 150°C, and N2 was purged and desorbed for 3 hours.
  • a fluorine-containing mixed gas 2% C 2 F 6 , 2% CF 4 , 2% CO 2 , 94% N 2
  • the desorbed PFCs were detected by a flue gas analyzer.
  • the adsorption amount of PFCs by the carbon material adsorbent was 1.75 mmol/g. It was also found that the desorbed carbon material was still very effective in purifying fluorine-containing gases when used as an adsorption material again.
  • a method for preparing porous carbon materials by modifying red mud and its application in adsorbing and treating fluorine-containing gases the specific steps are as follows:
  • Red mud from an aluminum company in Wenshan City, Yunnan province was placed in an oven at 100°C and dried to constant weight, and then ground to pass through a 100-mesh sieve to obtain red mud powder for use; then an appropriate amount of the red mud powder was taken into a beaker, and a 0.05 mol/L citric acid solution was added for acid treatment, wherein the citric acid in the citric acid solution accounted for 5% of the mass of the red mud powder to remove alkali metals and adhesive components in the red mud, and the red mud was placed in a magnetic stirrer and stirred at room temperature for 20 minutes at a speed of 300 rpm, and then filtered and washed with deionized water until the pH was neutral to obtain a red mud slurry for use;
  • step (3) The carbon material obtained in step (2) is added to the red mud slurry in a mass ratio of 1:2 with the red mud powder obtained in step (1), and the mixture is placed in a magnetic stirrer and stirred at room temperature for 2 h at a rotation speed of 300 rpm. After being fully mixed, the formed mixture is placed in a vacuum drying oven at 60°C for 12 h to remove moisture. The dried mixture is then placed in a tubular furnace under a N2 atmosphere, heated to 500°C at a heating rate of 5°C/min, and calcined for 3 h. After the calcination temperature is cooled to room temperature, a red mud-based porous carbon material is obtained.
  • the red mud-based porous carbon material was placed in a fixed bed reactor and pretreated at 300° C for 2h under N2 atmosphere. After cooling to 120°C, a fluorine-containing mixed gas (2% C2F6 , 2% CF4 , 2% CO2 , 94% N2 ) was introduced at a gas flow rate of 200mL/min for an adsorption experiment.
  • the outlet gas was detected for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, adsorption saturation was reached.
  • the temperature of the fixed bed reactor was then raised to 150°C, and N2 was purged and desorbed for 3h. The desorbed PFCs were detected by the flue gas analyzer.
  • the adsorption amount of PFCs by the carbon material adsorbent was 2.15mmol/g. It was also found that the desorbed carbon material was still very effective as an adsorbent material for purifying fluorine-containing gases.
  • a method for preparing porous carbon materials by modifying red mud and its application in adsorbing and treating fluorine-containing gases the specific steps are as follows:
  • Red mud from an aluminum company in Wenshan City, Yunnan province was placed in an oven and dried at 100°C to constant weight.
  • the red mud powder is ground and passed through a 100-mesh sieve to obtain a red mud powder for use; then an appropriate amount of the red mud powder is taken into a beaker, and a citric acid solution with a concentration of 0.05 mol/L is added for acid treatment, wherein the citric acid in the citric acid solution accounts for 10% of the mass of the red mud powder, and the alkali metal and adhesive components in the red mud are removed, and the red mud is placed in a magnetic stirrer and stirred at room temperature for 20 minutes at a speed of 300 rpm, and then filtered and washed with deionized water until the pH is neutral to obtain a red mud slurry for use;
  • step (3) The carbon material obtained in step (2) is added to the red mud slurry in a mass ratio of 1:2 with the red mud powder obtained in step (1), and the mixture is placed in a magnetic stirrer and stirred at room temperature for 2 h at a rotation speed of 300 rpm. After being fully mixed, the formed mixture is placed in a vacuum drying oven at 60°C for 12 h to remove moisture. The dried mixture is then placed in a tubular furnace under a N2 atmosphere, heated to 500°C at a heating rate of 5°C/min, and calcined for 3 h. After the calcination temperature is cooled to room temperature, a red mud-based porous carbon material is obtained.
  • the red mud-based porous carbon material was placed in a fixed bed reactor and pretreated at 300° C for 2h under N2 atmosphere. After cooling to 120°C, a fluorine-containing mixed gas (2% C2F6 , 2% CF4 , 2% CO2 , 94% N2 ) was introduced at a gas flow rate of 200mL/min for an adsorption experiment.
  • the outlet gas was detected for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, adsorption saturation was reached.
  • the temperature of the fixed bed reactor was then raised to 150°C, and N2 was purged and desorbed for 3h. The desorbed PFCs were detected by the flue gas analyzer. The adsorption amount of PFCs by the carbon material adsorbent was 2.45mmol/g. It was also found that the desorbed carbon material was still very effective as an adsorbent material for purifying fluorine-containing gases.
  • a method for preparing porous carbon materials by modifying red mud and its application in adsorbing and treating fluorine-containing gases the specific steps are as follows:
  • Red mud from an aluminum company in Wenshan City, Yunnan province was placed in an oven at 110° C. and dried to constant weight, and then ground to pass through a 100-mesh sieve to obtain red mud powder for use; then an appropriate amount of the red mud powder was taken into a beaker, and a 0.05 mol/L citric acid solution was added for acid treatment, wherein the citric acid in the citric acid solution accounted for 5% of the mass of the red mud powder to remove alkali metals and adhesive components in the red mud, and the red mud was placed in a magnetic stirrer and stirred at room temperature for 25 minutes at a speed of 400 rpm, and then filtered and washed with deionized water until the pH was neutral to obtain a red mud slurry for use;
  • step (3) The carbon material obtained in step (2) is added to the red mud slurry in a mass ratio of 1:3 to the red mud powder obtained in step (1), and the mixture is placed in a magnetic stirrer and stirred at room temperature for 3 hours at a rotation speed of 400 rpm. After sufficient mixing, the formed mixture is placed in a vacuum drying oven at 70°C for 12 hours to remove moisture. The dried mixture is then placed in a tubular furnace under a N2 atmosphere, and the temperature is increased to 500°C at a heating rate of 5°C/min and calcined for 3 hours. After the calcination temperature is cooled to room temperature, a red mud-based porous carbon material is obtained.
  • the red mud-based porous carbon material was placed in a fixed bed reactor and pretreated at 300° C for 2h under N2 atmosphere. After cooling to 120°C, a fluorine-containing mixed gas (2% C2F6 , 2% CF4 , 2% CO2 , 94% N2 ) was introduced at a gas flow rate of 200mL/min for an adsorption experiment.
  • the outlet gas was detected for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, adsorption saturation was reached.
  • the temperature of the fixed bed reactor was then raised to 150°C, and N2 was purged and desorbed for 3h. The desorbed PFCs were detected by the flue gas analyzer.
  • the adsorption amount of PFCs by the carbon material adsorbent was 2.48mmol/g. It was also found that the desorbed carbon material was still very effective as an adsorbent material for purifying fluorine-containing gases.
  • a method for preparing porous carbon materials by modifying red mud and its application in adsorbing and treating fluorine-containing gases the specific steps are as follows:
  • Red mud from an aluminum company in Wenshan City, Yunnan province was placed in an oven at 110° C. and dried to constant weight, and then ground to pass through a 100-mesh sieve to obtain red mud powder for use; then an appropriate amount of the red mud powder was taken into a beaker, and a 0.05 mol/L citric acid solution was added for acid treatment, wherein the citric acid in the citric acid solution accounted for 5% of the mass of the red mud powder to remove alkali metals and adhesive components in the red mud, and the red mud was placed in a magnetic stirrer and stirred at room temperature for 25 minutes at a speed of 400 rpm, and then filtered and washed with deionized water until the pH was neutral to obtain a red mud slurry for use;
  • step (3) The carbon material obtained in step (2) is added to the red mud slurry in a mass ratio of 1:4 to the red mud powder obtained in step (1), and the mixture is placed in a magnetic stirrer and stirred at room temperature for 3 h at a rotation speed of 400 rpm. After sufficient mixing, the formed mixture is placed in a vacuum drying oven at 70°C for 12 h to remove moisture. The dried mixture is then placed in a tubular furnace under a N2 atmosphere, and the temperature is increased to 500°C at a heating rate of 5°C/min and calcined for 3 h. After the calcination temperature is cooled to room temperature, a red mud-based porous carbon material is obtained.
  • the red mud-based porous carbon material was placed in a fixed bed reactor and pretreated at 300°C for 2 h under N 2 atmosphere. After cooling to 120°C, a fluorine-containing mixed gas (2% C 2 F 6 , 2% CF 4 , 2% CO 2 , 94% N 2 ) was introduced. The rate was 200mL/min, and the adsorption experiment was carried out. The outlet gas was detected for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, the adsorption saturation was reached. Then the temperature of the fixed bed reactor was increased to 150°C, and N2 was purged and desorbed for 3 hours. The desorbed PFCs were detected by the flue gas analyzer. The adsorption amount of PFCs by the carbon material adsorbent was 2.34mmol/g. At the same time, it was found that the desorbed carbon material was still very effective as an adsorption material for purifying fluorine-containing gases
  • a method for preparing porous carbon materials by modifying red mud and its application in adsorbing and treating fluorine-containing gases the specific steps are as follows:
  • Red mud from an aluminum company in Wenshan City, Yunnan province was placed in an oven at 115°C and dried to constant weight, and then ground to pass through a 100-mesh sieve to obtain red mud powder for use; then an appropriate amount of the red mud powder was taken into a beaker, and a citric acid solution with a concentration of 0.05 mol/L was added for acid treatment, wherein the citric acid in the citric acid solution accounted for 5% of the mass of the red mud powder to remove alkali metals and adhesive components in the red mud, and the red mud was placed in a magnetic stirrer and stirred at room temperature for 30 minutes at a speed of 500 rpm, and then filtered and washed with deionized water until the pH was neutral to obtain a red mud slurry for use;
  • step (3) The carbon material obtained in step (2) is added to the red mud slurry in a mass ratio of 1:3 with the red mud powder obtained in step (1) and mixed.
  • the mixture is placed in a magnetic stirrer at room temperature for 4 hours at a rotation speed of 500 rpm. After sufficient mixing, the formed mixture is placed in a vacuum drying oven at 80°C for 12 hours to remove moisture. The dried mixture is then placed in a tubular furnace under a N2 atmosphere and heated to 650°C at a heating rate of 5°C/min and calcined for 3 hours. After the calcination temperature is cooled to room temperature, a red mud-based porous carbon material is obtained.
  • the red mud-based porous carbon material was placed in a fixed bed reactor and pretreated at 300° C for 2h under N2 atmosphere. After cooling to 120°C, a fluorine-containing mixed gas (2% C2F6 , 2% CF4 , 2% CO2 , 94% N2 ) was introduced at a gas flow rate of 200mL/min for an adsorption experiment.
  • the outlet gas was detected for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, adsorption saturation was reached.
  • the temperature of the fixed bed reactor was then raised to 150°C, and N2 was purged and desorbed for 3h. The desorbed PFCs were detected by the flue gas analyzer. The adsorption amount of PFCs by the carbon material adsorbent was 2.54mmol/g. It was also found that the desorbed carbon material was still very effective as an adsorbent material for purifying fluorine-containing gases.
  • a method for preparing porous carbon material by modifying red mud and its application in adsorbing and treating fluorine-containing gas comprising the following steps: The steps are as follows:
  • Red mud from an aluminum company in Wenshan City, Yunnan province was placed in an oven at 115°C and dried to constant weight, and then ground to pass through a 100-mesh sieve to obtain red mud powder for use; then an appropriate amount of the red mud powder was taken into a beaker, and a citric acid solution with a concentration of 0.05 mol/L was added for acid treatment, wherein the citric acid in the citric acid solution accounted for 5% of the mass of the red mud powder to remove alkali metals and adhesive components in the red mud, and the red mud was placed in a magnetic stirrer and stirred at room temperature for 30 minutes at a speed of 500 rpm, and then filtered and washed with deionized water until the pH was neutral to obtain a red mud slurry for use;
  • step (3) The carbon material obtained in step (2) is added to the red mud slurry in a mass ratio of 1:3 with the red mud powder obtained in step (1), and the mixture is placed in a magnetic stirrer and stirred at room temperature for 4 hours at a rotation speed of 500 rpm. After being fully mixed, the formed mixture is placed in a vacuum drying oven at 80°C for 12 hours to remove moisture. The dried mixture is then placed in a tubular furnace under a N2 atmosphere, and the temperature is increased to 800°C at a heating rate of 5°C/min and calcined for 3 hours. After the calcination temperature is cooled to room temperature, a red mud-based porous carbon material is obtained.
  • the red mud-based porous carbon material was placed in a fixed bed reactor and pretreated at 300° C for 2h under N2 atmosphere. After cooling to 120°C, a fluorine-containing mixed gas (2% C2F6 , 2% CF4 , 2% CO2 , 94% N2 ) was introduced at a gas flow rate of 200mL/min for an adsorption experiment.
  • the outlet gas was detected for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, adsorption saturation was reached.
  • the temperature of the fixed bed reactor was then raised to 150°C, and N2 was purged and desorbed for 3h. The desorbed PFCs were detected by the flue gas analyzer. The adsorption amount of PFCs by the carbon material adsorbent was 1.90mmol/g. It was also found that the desorbed carbon material was still very effective as an adsorbent material for purifying fluorine-containing gases.
  • the red mud slurry prepared in Example 6 was filtered and placed in a vacuum drying oven at 80°C for 12h, then placed in a tubular furnace under N2 atmosphere, heated to 600°C at a heating rate of 5°C/min and calcined for 3h to obtain a red mud-based adsorbent, which was placed in a fixed bed reactor and pretreated at 300°C for 2h under N2 atmosphere.
  • a fluorine-containing mixed gas 2% C2F6 , 2% CF4 , 2% CO2 , 94% N2
  • the outlet gas was tested for PFCs using a flue gas analyzer.
  • the carbon material prepared in Example 6 was mixed with KOH with a concentration of 0.05 mol/L in a mass ratio of 1:3. The mixture was placed in a magnetic stirrer and stirred at room temperature for 1 h at a speed of 500 rpm. After being fully mixed, it was placed in a vacuum drying oven at 80°C for 12 h to remove moisture. The dried mixture was then placed in a tubular furnace under N2 atmosphere and heated to 650°C at a heating rate of 5°C/min for 3 h. After the calcination temperature was cooled to room temperature, a porous carbon material was obtained. The material was placed in a fixed bed reactor and pretreated at 300°C for 2 h under N2 atmosphere.
  • a fluorine - containing mixed gas (2% C2F6 , 2% CF4 , 2% CO2 , 94% N2 ) was introduced at a gas flow rate of 200 mL/min to conduct an adsorption experiment.
  • the outlet gas was tested for PFCs using a flue gas analyzer. When the outlet concentration was the same as the inlet concentration and no longer changed, adsorption saturation was reached.
  • the temperature of the fixed bed reactor was then raised to 150°C and N2 was conducted. 2 After purging and desorption for 3 hours, the desorbed PFCs were detected by flue gas analyzer, and the adsorption amount of PFCs by porous carbon material was 1.35mmol/g.
  • Example 1 Example 2, and Example 3, the effect of carbonization temperature on the performance of the adsorbent was considered, and 600°C was determined to be the optimal carbonization temperature of the carbon material; in Example 3, Example 4, and Example 5, the effect of the amount of red mud powder added on the performance of the adsorbent was considered. As the amount of red mud added increased, the adsorption effect of PFCs increased, but the adsorption effects of the carbon material and red mud powder mass ratios of 1:3 and 1:4 were similar, and considering the economic effect, 1:3 was the optimal mass ratio; in Example 4, Example 6, and Example 7, the effect of activation temperature on the performance of the adsorbent was considered.
  • the adsorption effect of PFCs decreased, because too high a temperature would cause the micropore volume and total specific surface area to decrease, which was not conducive to the adsorption of PFCs. Therefore, when the carbonization temperature was 600°C, the mass ratio of carbon material to red mud powder was 1:3, and the activation temperature was 650°C, that is, Example 6, the pore structure of the prepared red mud-based porous carbon adsorbent was richer, and the adsorption effect of PFCs was the best.

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  • Processing Of Solid Wastes (AREA)

Abstract

La présente invention concerne une méthode de préparation d'un matériau carboné poreux au moyen d'une modification de boue rouge et l'utilisation du matériau carboné poreux. La méthode comprend : la soumission de boue rouge à un séchage, un broyage, une lixiviation acide, un lavage, une filtration et un lavage pour obtenir une suspension de boue rouge neutre, le broyage et la carbonisation de bouteilles en plastique usagées, le mélange de celles-ci avec la suspension de boue rouge, la réalisation d'une agitation magnétique pour réaliser un mélange complet, et le séchage et l'activation du mélange boue rouge-matériau carboné formé, de façon à obtenir un matériau carboné poreux. Dans la présente invention, au moyen de méthodes de carbonisation et d'activation simples, des déchets solides industriels, c'est-à-dire de boue rouge, et de plastique sont convertis en un matériau adsorbant, un traitement gaz-solide coordonné est obtenu, et une nouvelle idée est fournie pour l'utilisation de ressources de la boue rouge ; par comparaison avec un adsorbant classique, le matériau carboné poreux, qui est préparé à partir de plastique carbonisé dopé avec de la boue rouge, dans la présente invention présente une meilleure structure de pores et une meilleure sélectivité ; de plus, les PFC peuvent être enrichis en un gaz à haute concentration après adsorption-désorption, et une certaine valeur économique est obtenue, de telle sorte qu'une utilisation respectueuse de l'environnement des déchets provenant de l'industrie de l'aluminium est obtenue, le coût de traitement environnemental est réduit, et les objectifs de réduction de la pollution, de réduction de carbone et d'interaction synergique sont obtenus.
PCT/CN2024/097780 2023-06-06 2024-06-06 Méthode de préparation d'un matériau carboné poreux au moyen d'une modification de boue rouge et utilisation d'un matériau carboné poreux Pending WO2024251202A1 (fr)

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