CN116654928A - Method for preparing porous carbon material by modifying red mud and application thereof - Google Patents
Method for preparing porous carbon material by modifying red mud and application thereof Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229920003023 plastic Polymers 0.000 claims abstract description 26
- 239000004033 plastic Substances 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000002699 waste material Substances 0.000 claims abstract description 15
- 230000004913 activation Effects 0.000 claims abstract description 9
- 238000003763 carbonization Methods 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 81
- 238000001179 sorption measurement Methods 0.000 claims description 54
- 239000000843 powder Substances 0.000 claims description 47
- 238000010438 heat treatment Methods 0.000 claims description 40
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 31
- 239000012298 atmosphere Substances 0.000 claims description 31
- 229910052731 fluorine Inorganic materials 0.000 claims description 31
- 239000011737 fluorine Substances 0.000 claims description 31
- 239000002002 slurry Substances 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 239000004698 Polyethylene Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 229920000573 polyethylene Polymers 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- -1 polyethylene Polymers 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 4
- PGSADBUBUOPOJS-UHFFFAOYSA-N neutral red Chemical compound Cl.C1=C(C)C(N)=CC2=NC3=CC(N(C)C)=CC=C3N=C21 PGSADBUBUOPOJS-UHFFFAOYSA-N 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 229920006926 PFC Polymers 0.000 abstract description 40
- 229910052799 carbon Inorganic materials 0.000 abstract description 23
- 239000003463 adsorbent Substances 0.000 abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011148 porous material Substances 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000002910 solid waste Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000002336 sorption--desorption measurement Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 52
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 19
- 239000003546 flue gas Substances 0.000 description 19
- 230000000694 effects Effects 0.000 description 16
- 229910002091 carbon monoxide Inorganic materials 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- 239000011363 dried mixture Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000010306 acid treatment Methods 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- 229910052783 alkali metal Inorganic materials 0.000 description 7
- 150000001340 alkali metals Chemical class 0.000 description 7
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000010792 warming Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000004131 Bayer process Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
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- 239000005431 greenhouse gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
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Classifications
-
- 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
Abstract
The invention discloses a method for preparing a porous carbon material by modifying red mud and application thereof. According to the invention, industrial solid waste red mud and plastic are converted into materials with adsorptivity by a simple carbonization and activation method, so that gas-solid cooperative treatment is realized, and a new idea is provided for recycling the red mud; compared with the traditional adsorbent, the porous carbon material prepared by using the red mud doped carbonized plastic has better pore structure and selectivity, and PFCs can be enriched into high-concentration gas after adsorption-desorption, so that the porous carbon material has certain economic value, thereby realizing the environment-friendly utilization of internal wastes in the aluminum industry, reducing the environmental treatment cost and achieving the aims of pollution reduction and carbon reduction synergy.
Description
Technical Field
The invention belongs to the technical field of solid waste resource utilization, and particularly relates to a method for preparing a porous carbon material by modifying red mud and application thereof.
Background
Red mud is used as a large amount of solid waste generated in the alumina production process, and can be classified into bayer process red mud, sintering process red mud and combination process red mud according to the quality and the production process of alumina. The red mud contains a large amount of Fe 2 O 3 、Al 2 O 3 And TiO 2 Such metal oxides have the potential to be an effective material for the treatment of atmospheric pollutants. The traditional treatment mode of red mud is mainly stockpiling, which not only occupies land resources, but also heavy metals in the red mud can infiltrate into the ground through surface water and rain water leaching to pollute surrounding soil, so that the soil is salted. Meanwhile, small particles on the surface of the red mud can also diffuse into the air, so that the air pollution is caused. Therefore, the improvement of the comprehensive utilization rate is a key for solving the problem of massive accumulation of the red mud.
Plastic is used as an organic polymer material, and is widely applied to industrial production and daily life due to the characteristics of convenient use, low cost, portability, high strength, corrosion resistance and the like. However, the plastic is easy to age and damage in the use process, has short service life and is difficult to degrade in natural environment, and white pollution can be caused if untreated waste plastic is directly discharged into the environment, thereby causing serious ecological crisis. The current treatment methods for plastics mainly comprise landfill, incineration and pyrolysis, wherein the landfill is the simplest method, but occupies a large amount of land resources; and a large amount of harmful gas is generated in the incineration process, and if the harmful gas leaks into the air, secondary pollution can be caused.
The industrial waste gas has great damage to the environment, great inconvenience is easily brought to the life of people, and the largest pollution source in the electrolytic aluminum industry is electrolysisThe fumes discharged from the tank, e.g. dust, perfluorocarbons (PFCs, mainly CF 4 And C 2 F 6 )、CO 2 Etc., wherein PFCs are strong greenhouse gases, have a longer lifetime and a higher global warming potential, the global warming potential being CO 2 Thousands or even tens of thousands of times, when discharged into the environment, are liable to cause global warming, resulting in problems such as glacier melting, sea level rise, land desertification, etc.
The emission reduction technology for PFCs at present mainly comprises combustion, cracking, catalysis and adsorption. Among them, adsorption is considered as a promising technique for capturing PFCs due to its low energy consumption, low cost, and ease of management. Among the adsorbents, porous carbon materials are widely used because of their advantages of low preparation cost, large specific surface area, developed pore structure, good chemical and mechanical stability, relative easy regeneration, and the like. Although a certain amount of pore structure can be obtained by treating the carbon material by using a physical or chemical activation manner in the conventional process of preparing the porous carbon material, the physical activation requires a very high temperature and a long time, the specific surface area of the activated carbon material is also relatively limited, and the chemically activated carbon material needs to be cleaned to remove the activator residues in the pore channels, thereby further increasing the cost of the reaction.
At present, the treatment of red mud and waste plastics in terms of adsorbents is mainly focused on preparing the adsorbents by treating the waste plastics with acid-base treatment red mud or an activating agent, and the materials prepared in the mode cannot fully utilize metal oxides, specific surface areas and pore structures contained in the materials, so that the efficient adsorption purification performance is difficult to realize, and the treatment aim of recycling the solid wastes is difficult to achieve.
Disclosure of Invention
The invention provides a method for preparing a porous carbon material and adsorbing fluorine-containing gas by combining red mud with plastic modification, which adopts a catalytic activation mode and utilizes abundant metal oxides such as Fe in the red mud 2 O 3 Doping with carbon material, activating, increasing the surface active point of micropores in the carbon material, and converting micropores into mesopores, thereby improving the adsorption effect of porous carbon adsorbent, and purifyingAnd (3) the effect of electrolytic aluminum smoke.
Meanwhile, in order to solve the problem of low utilization rate of red mud and plastics, the invention takes the red mud and the waste plastic bottles as raw materials, and the prepared porous carbon adsorbent has better adsorption property through simple carbonization and activation, so that PFCs in electrolytic aluminum flue gas can be removed, pollution of the red mud to the environment can be reduced, recycling of the red mud is realized, meanwhile, environmental protection utilization of waste in the aluminum industry is realized, environmental treatment cost is reduced, and the aim of reducing pollution and reducing carbon and synergy is fulfilled.
The technical scheme of the invention is as follows:
the method for preparing the porous carbon material by modifying the red mud comprises the following specific steps:
(1) Drying red mud at 100-115 ℃ to constant weight, grinding the dried red mud, sieving with a 100-mesh sieve to obtain red mud powder, adding citric acid solution with the concentration of 0.05mol/L into the red mud powder, magnetically stirring in a magnetic stirrer for 20-30min at room temperature, filtering, and washing with deionized water until the pH value is neutral to obtain neutral red mud slurry;
(2) Crushing the collected waste plastic bottles into small blocks and carbonizing to obtain a carbon material; mixing a carbon material with neutral red mud slurry, and magnetically stirring the mixture in a magnetic stirrer for 2-4 hours at room temperature;
(3) And (3) vacuum drying the mixture of the carbon material and the red mud slurry formed in the step (2), roasting and activating the dried material, and cooling to room temperature to obtain the red mud-based porous carbon material.
And (2) the citric acid in the citric acid solution in the step (1) accounts for 1-10% of the mass of the red mud powder.
The main component of the waste plastic bottle in the step (2) is Polyethylene (PE).
In the step (2), carbonization is performed in N 2 Heating to 450-600 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours.
The mass ratio of the carbon material in the step (2) to the red mud powder in the step (1) is 1:2-4.
The rotation speed of the magnetic stirrer in the step (1) and the step (2) is 300-500rpm.
In the step (3), the temperature of vacuum drying of the mixture of the carbon material and the red mud is 60-80 ℃ and the drying time is 12h.
In the step (3), the roasting activation is performed in N 2 And (3) heating to 500-800 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours.
The invention also provides an application of the red mud modified preparation porous carbon material in adsorbing fluorine-containing gas, wherein the porous carbon material is placed in a fixed bed reactor and is treated with N 2 Pretreating at 300 ℃ for 2 hours under the atmosphere, cooling to 120 ℃, introducing fluorine-containing gas, performing adsorption purification, heating to 150 ℃ for desorption after adsorption saturation, collecting desorbed gas, and using the desorbed carbon material as an adsorption material again for adsorption purification of the fluorine-containing gas.
The beneficial effects of the invention are as follows:
(1) Compared with the adsorption material prepared by singly utilizing red mud or waste plastics, the method has better effect, can not only improve the PFCs removal rate, but also reduce HF and CO 2 The gas is generated, and a new method is provided for the recycling of the red mud.
(2) After the PFCs are adsorbed by the porous carbon material prepared by the invention, the PFCs with high concentration can be obtained through adsorption-desorption, and the energy consumption in the subsequent treatment such as plasma decomposition and thermocatalysis processes can be reduced.
(3) According to the invention, the waste plastic bottles are converted into carbon materials to serve as carriers, and then the metal oxides in the red mud are loaded, so that the surface area of the materials and the selectivity of gas are enhanced, and the influence of waste plastics on the environment is relieved.
(4) The invention utilizes the method of treating waste with waste, not only improves the utilization rate of red mud and plastics, but also reduces the process cost and reduces the pollution to the environment.
Drawings
FIG. 1 is a process flow diagram of a porous carbon material modified by red mud to treat fluorine-containing gas.
Detailed Description
The present invention will be described in further detail with reference to the following examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. The reagents or apparatus used in the examples were conventional products available commercially without the manufacturer's knowledge.
The red mud used in the embodiment of the invention is from certain aluminum industry company in Wenshan city of Yunnan province.
Example 1
A method for preparing a porous carbon material by modifying red mud and application of adsorption treatment of fluorine-containing gas are shown in figure 1, and specifically comprise the following steps:
(1) Drying red mud from certain aluminum industry company in Wenshan, yunnan province in an oven at 100 ℃ to constant weight, grinding and sieving with a 100-mesh sieve to obtain red mud powder for later use; then taking a proper amount of red mud powder in a beaker, adding citric acid solution for acid treatment, wherein citric acid in the citric acid solution accounts for 1% of the mass of the red mud powder, removing alkali metal and adhesive components in the red mud, placing the red mud in a magnetic stirrer, stirring at room temperature for 20min at a rotating speed of 300rpm, filtering and washing with deionized water until pH is neutral, and obtaining red mud slurry for later use;
(2) Crushing the collected plastic bottle containing polyethylene into small pieces, placing in a tube furnace, and collecting N 2 Heating to 450 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours to obtain a carbon material;
(3) Adding the carbon material obtained in the step (2) into red mud slurry according to the mass ratio of 1:2 with the red mud powder obtained in the step (1), mixing, placing the mixture into a magnetic stirrer, stirring for 2 hours at room temperature at the speed of 300rpm, placing the formed mixture into a vacuum drying oven, drying at 60 ℃ for 12 hours after full mixing, removing water, and then placing the dried mixture into a tube furnace for N 2 And (3) in the atmosphere, heating to 500 ℃ at a heating rate of 5 ℃/min, and roasting for 3 hours, and cooling to room temperature after the roasting temperature is cooled to obtain the red mud-based porous carbon material.
Placing the red mud-based porous carbon material into a fixed bed reactor, and adding the red mud-based porous carbon material into N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And the desorption is carried out for 3 hours, the desorbed PFCs are detected by a flue gas analyzer, the adsorption capacity of the carbon material adsorbent to the PFCs is 1.75mmol/g, and meanwhile, the effect of purifying the fluorine-containing gas by taking the desorbed carbon material as an adsorption material is still good.
Example 2
A method for preparing a porous carbon material by modifying red mud and application of adsorbing fluorine-containing gas are specifically disclosed as follows:
(1) Drying red mud from certain aluminum industry company in Wenshan, yunnan province in an oven at 100 ℃ to constant weight, grinding and sieving with a 100-mesh sieve to obtain red mud powder for later use; then taking a proper amount of red mud powder in a beaker, adding 0.05mol/L citric acid solution for acid treatment, wherein the citric acid in the citric acid solution accounts for 5% of the mass of the red mud powder, removing alkali metal and adhesive components in the red mud, placing the red mud powder in a magnetic stirrer, stirring for 20min at room temperature at the rotating speed of 300rpm, filtering and washing with deionized water until the pH is neutral, and obtaining red mud slurry for later use;
(2) Breaking the collected polyethylene plastic bottle into small pieces, and placing in a tube furnace 2 Heating to 525 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours to obtain a carbon material;
(3) Adding the carbon material obtained in the step (2) into red mud slurry according to the mass ratio of 1:2 with the red mud powder obtained in the step (1), mixing, placing the mixture into a magnetic stirrer, stirring for 2 hours at room temperature at the speed of 300rpm, placing the formed mixture into a vacuum drying oven, drying at 60 ℃ for 12 hours after full mixing, removing water, and then placing the dried mixture into a tube furnace for N 2 And (3) in the atmosphere, heating to 500 ℃ at a heating rate of 5 ℃/min, and roasting for 3 hours, and cooling to room temperature after the roasting temperature is cooled to obtain the red mud-based porous carbon material.
Will be redThe mud-based porous carbon material is placed in a fixed bed reactor and is treated by a catalyst in N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And the desorption is carried out for 3 hours, the desorbed PFCs are detected by a flue gas analyzer, the adsorption capacity of the carbon material adsorbent to the PFCs is 2.15mmol/g, and meanwhile, the effect of purifying the fluorine-containing gas by taking the desorbed carbon material as an adsorption material is still good.
Example 3
A method for preparing a porous carbon material by modifying red mud and application of adsorbing fluorine-containing gas are specifically disclosed as follows:
(1) Drying red mud from certain aluminum industry company in Wenshan, yunnan province in an oven at 100 ℃ to constant weight, grinding and sieving with a 100-mesh sieve to obtain red mud powder for later use; then taking a proper amount of red mud powder in a beaker, adding citric acid solution with the concentration of 0.05mol/L for acid treatment, wherein citric acid in the citric acid solution accounts for 10% of the mass of the red mud powder, removing alkali metal and adhesive components in the red mud, placing the red mud powder in a magnetic stirrer, stirring for 20min at room temperature at the rotating speed of 300rpm, filtering, and washing with deionized water until the pH is neutral to obtain red mud slurry for later use;
(2) Breaking the collected polyethylene plastic bottle into small pieces, and placing in a tube furnace 2 Heating to 600 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours to obtain a carbon material;
(3) Adding the carbon material obtained in the step (2) into red mud slurry according to the mass ratio of 1:2 with the red mud powder obtained in the step (1), mixing, placing the mixture into a magnetic stirrer, stirring for 2 hours at room temperature at the speed of 300rpm, placing the formed mixture into a vacuum drying oven, drying at 60 ℃ for 12 hours after fully mixing, removing water, and placing the dried mixture into a tube typeN in furnace 2 And (3) in the atmosphere, heating to 500 ℃ at a heating rate of 5 ℃/min, and roasting for 3 hours, and cooling to room temperature after the roasting temperature is cooled to obtain the red mud-based porous carbon material.
Placing the red mud-based porous carbon material into a fixed bed reactor, and adding the red mud-based porous carbon material into N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And the desorption is carried out for 3 hours, the desorbed PFCs are detected by a flue gas analyzer, the adsorption capacity of the carbon material adsorbent to the PFCs is 2.45mmol/g, and meanwhile, the effect of purifying the fluorine-containing gas by taking the desorbed carbon material as an adsorption material is still good.
Example 4
A method for preparing a porous carbon material by modifying red mud and application of adsorbing fluorine-containing gas are specifically disclosed as follows:
(1) Drying red mud from certain aluminum industry company in Wenshan, yunnan province in an oven at 110 ℃ to constant weight, grinding and sieving with a 100-mesh sieve to obtain red mud powder for later use; then taking a proper amount of red mud powder in a beaker, adding citric acid solution with the concentration of 0.05mol/L for acid treatment, wherein citric acid in the citric acid solution accounts for 5% of the mass of the red mud powder, removing alkali metal and adhesive components in the red mud, placing the red mud powder in a magnetic stirrer, stirring for 25min at room temperature at the rotating speed of 400rpm, filtering, and washing with deionized water until the pH is neutral to obtain red mud slurry for later use;
(2) Breaking the collected polyethylene plastic bottle into small pieces, and placing in a tube furnace 2 Heating to 600 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours to obtain a carbon material;
(3) Adding the carbon material obtained in the step (2) into red mud slurry according to the mass ratio of the carbon material to the red mud powder obtained in the step (1) of 1:3, and mixing the mixtureStirring in a magnetic stirrer at room temperature for 3 hr at 400rpm, mixing thoroughly, drying at 70deg.C in a vacuum drying oven for 12 hr, removing water, and placing the dried mixture in a tube furnace for N 2 And (3) in the atmosphere, heating to 500 ℃ at a heating rate of 5 ℃/min, and roasting for 3 hours, and cooling to room temperature after the roasting temperature is cooled to obtain the red mud-based porous carbon material.
Placing the red mud-based porous carbon material into a fixed bed reactor, and adding the red mud-based porous carbon material into N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And the desorption is carried out for 3 hours, the desorbed PFCs are detected by a flue gas analyzer, the adsorption capacity of the carbon material adsorbent to the PFCs is 2.48mmol/g, and meanwhile, the effect of purifying the fluorine-containing gas by taking the desorbed carbon material as an adsorption material is still good.
Example 5
A method for preparing a porous carbon material by modifying red mud and application of adsorbing fluorine-containing gas are specifically disclosed as follows:
(1) Drying red mud from certain aluminum industry company in Wenshan, yunnan province in an oven at 110 ℃ to constant weight, grinding and sieving with a 100-mesh sieve to obtain red mud powder for later use; then taking a proper amount of red mud powder in a beaker, adding 0.05mol/L citric acid solution for acid treatment, wherein the citric acid in the citric acid solution accounts for 5% of the mass of the red mud powder, removing alkali metal and adhesive components in the red mud, placing the red mud powder in a magnetic stirrer, stirring the red mud powder at room temperature for 25min at the rotating speed of 400rpm, filtering and washing the red mud powder by using deionized water until the pH is neutral, and obtaining red mud slurry for later use;
(2) Breaking the collected polyethylene plastic bottle into small pieces, and placing in a tube furnace 2 Heating to 600 ℃ at a heating rate of 5 ℃/min under the atmosphere, roasting for 3 hours,obtaining a carbon material;
(3) Adding the carbon material obtained in the step (2) into red mud slurry according to the mass ratio of 1:4 with red mud powder obtained in the step (1), mixing, placing the mixture into a magnetic stirrer, stirring for 3 hours at room temperature at 400rpm, placing the formed mixture into a vacuum drying oven, drying at 70 ℃ for 12 hours after full mixing, removing water, and then placing the dried mixture into a tube furnace for N 2 And (3) in the atmosphere, heating to 500 ℃ at a heating rate of 5 ℃/min, and roasting for 3 hours, and cooling to room temperature after the roasting temperature is cooled to obtain the red mud-based porous carbon material.
Placing the red mud-based porous carbon material into a fixed bed reactor, and adding the red mud-based porous carbon material into N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And the desorption is carried out for 3 hours, the desorbed PFCs are detected by a flue gas analyzer, the adsorption capacity of the carbon material adsorbent to the PFCs is 2.34mmol/g, and meanwhile, the effect of purifying the fluorine-containing gas by taking the desorbed carbon material as an adsorption material is still good.
Example 6
A method for preparing a porous carbon material by modifying red mud and application of adsorbing fluorine-containing gas are specifically disclosed as follows:
(1) Drying red mud from certain aluminum industry company in Wenshan, yunnan province in 115 ℃ in an oven until the weight is constant, and grinding the red mud through a 100-mesh sieve to obtain red mud powder for later use; then taking a proper amount of red mud powder in a beaker, adding citric acid solution with the concentration of 0.05mol/L for acid treatment, wherein citric acid in the citric acid solution accounts for 5% of the mass of the red mud powder, removing alkali metal and adhesive components in the red mud, placing the red mud powder in a magnetic stirrer, stirring for 30min at room temperature at the rotating speed of 500rpm, filtering, and washing with deionized water until the pH is neutral to obtain red mud slurry for later use;
(2) Breaking the collected polyethylene plastic bottle into small pieces, and placing in a tube furnace 2 Heating to 600 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours to obtain a carbon material;
(3) Adding the carbon material obtained in the step (2) into red mud slurry according to the mass ratio of the carbon material to the red mud powder obtained in the step (1) of 1:3, mixing, placing the mixture into a magnetic stirrer for 4 hours at room temperature at 500rpm, placing the formed mixture into a vacuum drying oven for drying at 80 ℃ for 12 hours after fully mixing, removing water, and then placing the dried mixture into a tube furnace for N 2 And (3) in the atmosphere, heating to 650 ℃ at a heating rate of 5 ℃/min, and roasting for 3 hours, and cooling to room temperature after the roasting temperature is cooled to obtain the red mud-based porous carbon material.
Placing the red mud-based porous carbon material into a fixed bed reactor, and adding the red mud-based porous carbon material into N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And the desorption is carried out for 3 hours, the desorbed PFCs are detected by a flue gas analyzer, the adsorption capacity of the carbon material adsorbent to the PFCs is 2.54mmol/g, and meanwhile, the effect of purifying the fluorine-containing gas by taking the desorbed carbon material as an adsorption material is still good.
Example 7
A method for preparing a porous carbon material by modifying red mud and application of adsorbing fluorine-containing gas are specifically disclosed as follows:
(1) Drying red mud from certain aluminum industry company in Wenshan, yunnan province in 115 ℃ in an oven until the weight is constant, and grinding the red mud through a 100-mesh sieve to obtain red mud powder for later use; then taking a proper amount of red mud powder in a beaker, adding citric acid solution with the concentration of 0.05mol/L for acid treatment, wherein citric acid in the citric acid solution accounts for 5% of the mass of the red mud powder, removing alkali metal and adhesive components in the red mud, placing the red mud powder in a magnetic stirrer, stirring for 30min at room temperature at the rotating speed of 500rpm, filtering, and washing with deionized water until the pH is neutral to obtain red mud slurry for later use;
(2) Breaking the collected polyethylene plastic bottle into small pieces, and placing in a tube furnace 2 Heating to 600 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours to obtain a carbon material;
(3) Adding the carbon material obtained in the step (2) into red mud slurry according to the mass ratio of the carbon material to the red mud powder obtained in the step (1) of 1:3, mixing, placing the mixture into a magnetic stirrer, stirring for 4 hours at room temperature at the speed of 500rpm, placing the formed mixture into a vacuum drying oven, drying at 80 ℃ for 12 hours after the mixture is fully mixed, removing water, and then placing the dried mixture into a tubular furnace for N 2 And (3) in the atmosphere, heating to 800 ℃ at a heating rate of 5 ℃/min, roasting for 3 hours, and cooling to room temperature after the roasting temperature is cooled to obtain the red mud-based porous carbon material.
Placing the red mud-based porous carbon material into a fixed bed reactor, and adding the red mud-based porous carbon material into N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And the desorption is carried out for 3 hours, the desorbed PFCs are detected by a flue gas analyzer, the adsorption capacity of the carbon material adsorbent to the PFCs is 1.90mmol/g, and meanwhile, the effect of purifying the fluorine-containing gas by taking the desorbed carbon material as an adsorption material is still good.
Comparative example 1
Filtering the red mud slurry prepared in the example 6, placing the filtered red mud slurry in a vacuum drying oven for drying at 80 ℃ for 12 hours, and then placing the dried red mud slurry in a tube furnace for N 2 Roasting for 3 hours at the temperature rising rate of 5 ℃/min to 600 ℃ under the atmosphere to obtain the red mud-based adsorbent, and placing the red mud-based adsorbent in a fixed bed reactor, and adding the red mud-based adsorbent into a reaction vessel 2 Pretreatment at 300℃under an atmosphere 2h, cooling to 120 ℃, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And (3) purging and desorbing for 3 hours, wherein the desorbed PFCs are detected by a flue gas analyzer, and the adsorption quantity of the red mud-based adsorbent on the PFCs is 1.12mmol/g.
Comparative example 2
Mixing the carbon material prepared in example 6 with KOH with the concentration of 0.05mol/L according to the mass ratio of 1:3, stirring the mixture in a magnetic stirrer at room temperature for 1h at the rotation speed of 500rpm, fully mixing, drying at 80 ℃ in a vacuum drying oven for 12h, removing water, and then placing the dried mixture in a tubular furnace for N 2 In the atmosphere, heating to 650 ℃ at a heating rate of 5 ℃/min for roasting for 3 hours, cooling to room temperature after roasting temperature, obtaining a porous carbon material, placing the porous carbon material in a fixed bed reactor, and adding the porous carbon material into N 2 Pretreating at 300deg.C for 2 hr under atmosphere, cooling to 120deg.C, and introducing fluorine-containing mixed gas (2% C) 2 F 6 ，2％CF 4 、2％CO 2 、94％N 2 ) The gas flow rate is 200mL/min, adsorption experiments are carried out, the outlet gas is used for detecting PFCs by a flue gas analyzer, when the outlet concentration and the inlet concentration are the same and are not changed any more, adsorption saturation is achieved, then the temperature of the fixed bed reactor is increased to 150 ℃, and N is carried out 2 And (3) purging and desorbing for 3 hours, wherein the desorbed PFCs are detected by a flue gas analyzer, and the adsorption quantity of the porous carbon material to the PFCs is 1.35mmol/g.
Example 1, example 2, example 3, taking into account the effect of carbonization temperature on the adsorbent performance, determined the optimum carbonization temperature for a carbon material at 600 ℃; in the embodiment 3, the embodiment 4 and the embodiment 5, the influence of the addition amount of the red mud powder on the performance of the adsorbent is considered, the adsorption effect of the PFCs is increased along with the increase of the addition amount of the red mud, but the adsorption effects of the carbon material and the red mud powder are similar in mass ratio of 1:3 to 1:4, and the economic effect is considered, namely, the mass ratio of 1:3 is the optimal mass ratio; examples 4, 6 and 7 consider the influence of the activation temperature on the performance of the adsorbent, and the adsorption effect of PFCs decreases with increasing temperature, because too high a temperature results in a decrease in micropore volume and total specific surface area, which is detrimental to the adsorption of PFCs. Therefore, when the carbonization temperature is 600 ℃, the mass ratio of the carbon material to the red mud powder is 1:3, and the activation temperature is 650 ℃, namely, the prepared red mud-based porous carbon adsorbent has a richer pore structure and has the best adsorption effect on PFCs.
Claims (9)
1. The method for preparing the porous carbon material by modifying the red mud is characterized by comprising the following specific steps of:
(1) Drying red mud at 100-115 ℃ to constant weight, grinding the dried red mud, sieving with a 100-mesh sieve to obtain red mud powder, adding citric acid solution with the concentration of 0.05mol/L into the red mud powder, magnetically stirring at room temperature for 20-30min, filtering, and washing with deionized water until the pH value is neutral to obtain neutral red mud slurry;
(2) Crushing the collected waste plastic bottles into small blocks for carbonization to obtain a carbon material; mixing a carbon material with neutral red mud slurry, and magnetically stirring the mixture at room temperature for 2-4h;
(3) And (3) vacuum drying the mixture of the carbon material and the red mud slurry formed in the step (2), roasting and activating the dried material, and cooling to room temperature to obtain the red mud-based porous carbon material.
2. The method for preparing the porous carbon material by modifying the red mud according to claim 1, wherein the citric acid in the citric acid solution in the step (1) accounts for 1-10% of the mass of the red mud powder.
3. The method for preparing the porous carbon material by modifying red mud according to claim 1, wherein the main component of the waste plastic bottle in the step (2) is polyethylene.
4. The method for preparing the porous carbon material by modifying red mud according to claim 1, wherein the carbonization in the step (2) is performed byN 2 Heating to 450-600 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours.
5. The method for preparing the porous carbon material by modifying the red mud according to claim 1, wherein the mass ratio of the carbon material in the step (2) to the red mud powder in the step (1) is 1:2-4.
6. The method for preparing the porous carbon material by modifying red mud according to claim 1, wherein the rotation speed of the magnetic stirring in the step (1) and the step (2) is 300-500rpm.
7. The method for preparing the porous carbon material by modifying red mud according to claim 1, wherein the mixture in the step (3) is dried in vacuum at 60-80 ℃ for 12 hours.
8. The method for preparing the porous carbon material by modifying red mud according to claim 1, wherein the roasting activation in the step (3) is performed in the presence of N 2 And (3) heating to 500-800 ℃ at a heating rate of 5 ℃/min under the atmosphere, and roasting for 3 hours.
9. The method for preparing porous carbon material by modifying red mud as claimed in claim 1, wherein the porous carbon material is placed in a fixed bed reactor and treated with fluorine-containing gas under N 2 Pretreating at 300 ℃ for 2 hours under the atmosphere, cooling to 120 ℃, introducing fluorine-containing gas, performing adsorption purification, heating to 150 ℃ for desorption after adsorption saturation, collecting desorbed gas, and using the desorbed carbon material as an adsorption material again for adsorption purification of the fluorine-containing gas.
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| CN106881019A (en) * | 2017-02-23 | 2017-06-23 | 中国矿业大学 | A kind of method that utilization red mud and activated carbon thermal activation prepare desulfurizing agent |
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| CN109809404A (en) * | 2019-04-04 | 2019-05-28 | 安徽工业大学 | A kind of Bayer process red mud modification biological activated carbon and preparation method thereof for degradation of formaldehyde |
| CN111389347A (en) * | 2020-04-09 | 2020-07-10 | 中国铝业股份有限公司 | Wastewater defluorination adsorbent and preparation method thereof |
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| CN106881019A (en) * | 2017-02-23 | 2017-06-23 | 中国矿业大学 | A kind of method that utilization red mud and activated carbon thermal activation prepare desulfurizing agent |
| CN109626486A (en) * | 2018-12-29 | 2019-04-16 | 西安交通大学 | A kind of method of coupling processing high concentrated organic wastewater and heavy metal wastewater thereby |
| CN109809404A (en) * | 2019-04-04 | 2019-05-28 | 安徽工业大学 | A kind of Bayer process red mud modification biological activated carbon and preparation method thereof for degradation of formaldehyde |
| CN111389347A (en) * | 2020-04-09 | 2020-07-10 | 中国铝业股份有限公司 | Wastewater defluorination adsorbent and preparation method thereof |
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