CN115849510A - Method for preparing particle electrode by using gasification furnace slag and application - Google Patents
Method for preparing particle electrode by using gasification furnace slag and application Download PDFInfo
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- CN115849510A CN115849510A CN202111124187.2A CN202111124187A CN115849510A CN 115849510 A CN115849510 A CN 115849510A CN 202111124187 A CN202111124187 A CN 202111124187A CN 115849510 A CN115849510 A CN 115849510A
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- 238000001994 activation Methods 0.000 claims abstract description 16
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- 238000011282 treatment Methods 0.000 claims abstract description 14
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- 238000010306 acid treatment Methods 0.000 claims abstract description 5
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- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
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Abstract
The invention discloses a preparation method of a particle electrode, which takes gasification furnace slag as a raw material, and obtains modified gasification furnace slag after alkali treatment, activation and acid treatment, the modified gasification furnace slag is mixed and roasted with clay, a foaming agent and a pore-forming agent to obtain the particle electrode, and the modified gasification furnace slag, the clay, the foaming agent and the pore-forming agent comprise the following components in percentage by weight: 60-88% of gasification furnace slag, 10-30% of clay, 1-10% of foaming agent and 1-10% of pore-forming agent. The preparation method is simple, has low cost, can improve the electrochemical and catalytic activity and stability of the three-dimensional electrode, belongs to a novel green and safe technology for 'treating wastes with wastes', and has good economic and environmental benefits and optimistic industrial application and popularization prospects.
Description
Technical Field
The invention relates to a utilization method of gasification furnace slag, in particular to a method for preparing a particle electrode by utilizing the gasification furnace slag and application thereof.
Background
The three-dimensional electrode is also called a bed electrode, and refers to a three-dimensional electrode reactor formed by filling granular or chip-shaped materials between traditional two-dimensional electrode plates. Granular or chip-shaped materials form the particle electrode, and under proper electric field intensity, the particles can be polarized into a micro battery with one end being positively charged and the other end being negatively charged, so that the electrode area is greatly increased, and compared with the traditional two-dimensional electrode, the three-dimensional electrode has a better degradation effect on pollutants. Among the three-dimensional electrocatalytic reactors of repolarization, the choice of particle electrodes is one of the most important factors affecting the catalytic effect. The active carbon particle electrode is widely applied due to good adsorption performance and low price, but the mass transfer efficiency of pollutants is accelerated only through strong adsorption performance, the active carbon particle electrode does not participate in pollutant degradation reaction, the electrolysis time required for the pollutants to achieve the expected degradation effect is longer, the energy consumption is higher, and in order to reduce the energy consumption, if a chemical agent with a catalytic action is added in the electrolysis process, the difficulty of separating the chemical agent in the subsequent wastewater treatment process can be increased. CN106064926A discloses a method for preparing a catalytic particle electrode by utilizing sludge and fly ash. The three-dimensional electrode particle electrode is prepared by adopting sewage sludge and fly ash as raw materials through the steps of doping and dipping, microwave high-temperature activation, acid washing, screening and the like, but has the problems of low specific surface area and low strength, thereby causing low current efficiency and poor long-term use stability. CN103951018A discloses a multidimensional electro-Fenton device and a method for treating industrial sewage by using the same. The iron-carbon alloy is used as a particle electrode, the mass transfer efficiency is improved by a circulating pump, the circulating water amount is 2-6 times of the treated water amount, the particle electrode disclosed in the patent application has higher current efficiency, but iron is dissolved out under the action of an electric field due to higher iron content in an iron-carbon material, iron mud is attached to the surface of the filler, and the problems of filler hardening and overlarge short-circuit current after long-time use exist.
On the other hand, the industrial production of China generates a large amount of solid wastes every year, and if the wastes are not properly treated, the wastes are not only a resourceIs wasteful and also severely impacts the ecological environment. The slag product of gasification furnace slag gasified coal is a solid slag residue after controlling coal to be gasified after heating and burning in the gasification furnace, the physical components of the gasification and calcination furnace slag are mainly influenced by the structural composition of raw furnace coal, the ash content and the sulfur content, the raw coal gasification and calcination process and other factors, and the gasification furnace slag gasified coal is mainly composed of gasification SiO and AlO 3 CaO, gasified carbon residue and the like, and belongs to general solid waste. The main treatment method at present is to pile up the slag, which not only occupies a large amount of farmland, but also seriously pollutes the environment. The gasification slag contains a certain amount of metallic elements in addition to non-metallic elements. According to research literature, the main chemical elements contained in the slag are oxygen, silicon, calcium, aluminum, iron, magnesium and the like, and the elements mainly exist in the form of compounds. If the slag can be recycled, not only can the resource utilization of industrial waste be realized, but also the environmental pollution can be reduced. Slag has long been used as a building material, for example: paving roads, building bridges, building houses, etc. In recent years, researchers have utilized the adsorption characteristics of slag to remove substances such as phosphate, ammonia nitrogen and arsenic from water. Currently, the concept of "treating waste with waste" is of great interest in the field of water treatment, and therefore slag can be used in the field of water treatment. The electrochemical oxidation technology can rapidly decompose and oxidize organic pollutants in water into small molecular substances and further thoroughly convert the organic pollutants into CO 2 Water and inorganic salts, etc., have been widely used in the research of refractory organic pollutants. The slag is used as an electrode material in electrochemical sewage treatment, so that the slag can be fully reused, and the problem of the cost of a particle electrode can be solved.
However, the slag has the problems of small specific surface area and low activity, and needs to be matched with a carbon material for use, so that the catalytic action of the particle electrode is influenced, and the preparation cost and the manufacturing cost are increased by adding active metal.
Disclosure of Invention
Aiming at the problems in the preparation process of the particle electrode, the invention provides a novel preparation method of the particle electrode, which does not need to add an iron-carbon material additionally, further simplifies the preparation process, improves the specific surface area and the activity of the particle electrode, and improves the removal efficiency of COD when the particle electrode is used for sewage treatment in a three-dimensional electrode reactor.
In order to solve the above technical problems, a first aspect of the present invention provides a method for preparing a particle electrode, wherein a modified gasification furnace slag is obtained by using gasification furnace slag as a raw material and performing alkali treatment, activation and acid treatment, the modified gasification furnace slag is mixed with clay, a foaming agent and a pore-forming agent and is roasted to obtain the particle electrode, and the weight content of each component is as follows based on the weight of the particle electrode: 60-88% of gasification furnace slag, 10-30% of clay, 1-10% of foaming agent and 1-10% of pore-forming agent; preferably, the weight contents of the components are as follows: 65-75% of gasification furnace slag, 15-25% of clay, 3-8% of foaming agent and 3-8% of pore-forming agent.
Further, in the above technical solution, before the alkali treatment of the gasification furnace slag, it is preferable to perform a drying treatment. Further preferably dried at 100-120 deg.C for 2-5h.
Further, in the above technical scheme, the alkali treatment is to mix and grind the gasification furnace slag and carbonate, preferably sodium carbonate or potassium carbonate, until the mixture is uniform.
Further, in the technical scheme, the mass ratio of the gasification furnace slag to the carbonate is 100 (5-20); preferably, the mass ratio of the gasification slag to the carbonate is 100 (5-10).
Further, in the above technical scheme, the gasification furnace slag in step 1) is taken from the gasification furnace coarse slag.
Further, in the above technical solution, the activation conditions are: the activation temperature is 500-750 ℃, the activation time is 1-4h, and nitrogen is adopted for protection in the activation process; preferably, the activation temperature is 600-700 ℃ and the activation time is 2-3h.
Further, in the above technical scheme, the acid treatment is: soaking with acid solution with concentration of 2-4mol/L for 2-4h; preferably, the concentration of the acid solution is 2-3mol/L, and the soaking time is 2.5-3.5h. The acid is preferably one or more of hydrochloric acid, sulfuric acid or nitric acid.
Further, in the above technical solution, the foaming agent is selected from one or more of iron oxide, magnesium carbonate, silicon carbide and the like; the pore-forming agent is selected from one or more of starch, plant straw and the like.
Further, in the above technical scheme, the roasting conditions are as follows: the roasting temperature is 800-1000 ℃, and the roasting time is 2-4h; preferably, the roasting temperature is 850-950 ℃, and the roasting time is 2-3h.
Further, in the above technical scheme, preferably, the mixing is followed by molding and drying, wherein the molding is to add water to the mixed materials to prepare 30-50mm pellets. The drying comprises the following steps: drying at 80-150 deg.C for 1-5h.
The second aspect of the invention provides an application of the particle electrode prepared by any one of the methods in treating wastewater by using a three-dimensional electrode reactor.
Further, in the above technical scheme, the anode of the three-dimensional electrode reactor is a titanium-based coating electrode, the cathode is a graphite electrode, and the filler is the particle electrode prepared by the method of the present invention, wherein the loading amount of the particle electrode is not less than 50%.
Further, in the technical scheme, the three-dimensional electrode reactor is provided with an aeration device which can aerate the inside of the reactor, and the aeration rate is preferably 30-150L/h.
Further, in the above technical solution, the operating conditions of the three-dimensional electrode are as follows: the voltage of the three-dimensional electrode reactor is 5-20V, and the retention time is 30-120 min.
The invention has the following beneficial effects:
1. the material basis of the catalytic particle electrode prepared by the invention is waste gasification furnace slag, the preparation cost of the particle electrode is greatly reduced, the problems of harmlessness and high value-added utilization of the waste are effectively solved, and the catalytic particle electrode has good economic and environmental benefits.
2. The catalytic particle electrode prepared by the invention not only greatly increases the area of the electrochemical reaction working electrode and improves the current efficiency and the space utilization rate of a reaction system, but also can catalyze electro-Fenton to decompose H because the gasification furnace slag contains a large amount of metal oxides such as Fe, al and the like 2 O 2 Generating oxidation energyStronger free radicals, and the overall treatment efficiency of the reaction system is improved without adding additional chemical agents.
3. When the three-dimensional electrode reactor adopting the particle electrode is used for treating wastewater, the removal efficiency of COD can be obviously improved.
The preparation method is simple, has low cost, can improve the electrochemical and catalytic activity and stability of the three-dimensional electrode, belongs to a novel green and safe technology for 'treating wastes with wastes', and has good economic and environmental benefits and optimistic industrial application and popularization prospects.
Detailed Description
The present invention is further illustrated by the following examples, which are to be construed as merely illustrative and not a limitation of the scope.
[ example 1 ]
Grinding 120g of dried gasification furnace slag and 8.4g of sodium carbonate until the mixture is uniformly mixed, placing the mixture in a tubular heating furnace, activating the mixture for 2 hours at 700 ℃ in the atmosphere of nitrogen, cooling the mixture to room temperature along with the furnace, adding 90mL of 3mol/L hydrochloric acid, soaking the mixture for 3 hours, and drying the mixture to obtain the modified gasification furnace slag. Taking 70g of modified gasification furnace slag, 20g of clay, 5g of ferric oxide and 5g of starch, uniformly mixing, adding water to prepare small balls of 30-50mm, drying at 110 ℃ for 2h, roasting the dried small balls in a muffle furnace at 900 ℃ for 2h, and cooling to obtain the three-dimensional electrode catalytic particle electrode.
The catalytic particle electrode is arranged in a three-dimensional electrode reactor with a titanium-based coating electrode as an anode and a graphite electrode as a cathode, and the filling amount is 60 percent. Under the conditions of 15V voltage, 60min retention time and 90L/h aeration rate, oily sewage with the COD concentration of 1820mg/L is introduced, the COD removal rate after 2h is 87.2 percent, and the COD removal rate after 30h is 85.4 percent.
[ example 2 ]
Grinding 42g of dried gasification furnace slag and 8.4g of sodium carbonate until the materials are uniformly mixed, placing the mixture in a tubular heating furnace, activating the mixture for 3 hours at 600 ℃ in a nitrogen atmosphere, cooling the mixture to room temperature along with the furnace, adding 90mL of 2mol/L hydrochloric acid, soaking the mixture for 4 hours, and drying the mixture to obtain the modified gasification furnace slag. And (2) uniformly mixing 80g of modified gasification furnace slag, 15g of clay, 2g of ferric oxide and 3g of starch, adding water to prepare small balls with the diameter of 30-50mm, drying at 110 ℃ for 2h, roasting the dried small balls in a muffle furnace at 800 ℃ for 2h, and cooling to obtain the three-dimensional electrode catalytic particle electrode.
The catalytic particle electrode is arranged in a three-dimensional electrode reactor with a titanium-based coating electrode as an anode and a graphite electrode as a cathode, and the loading amount is 70%. Under the conditions of 15V voltage, 60min retention time and 90L/h aeration rate, oily sewage with the COD concentration of 1820mg/L is introduced, the COD removal rate after 2h is 75.5 percent, and the COD removal rate after 30h is 74.2 percent.
[ example 3 ]
Grinding 84g of dried gasification furnace slag and 8.4g of sodium carbonate until the materials are uniformly mixed, placing the mixture in a tubular heating furnace, activating the mixture for 4 hours at 550 ℃ in a nitrogen atmosphere, cooling the mixture to room temperature along with the furnace, adding 90mL of 4mol/L hydrochloric acid, soaking the mixture for 3 hours, and drying the mixture to obtain the modified gasification furnace slag. Taking 65g of modified gasification furnace slag, 25g of clay, 2.5g of magnesium carbonate and 7.5g of corn straw, uniformly mixing, adding water to prepare small balls of 30-50mm, drying at 110 ℃ for 2h, roasting the dried small balls in a muffle furnace at 1000 ℃ for 2h, and cooling to obtain the three-dimensional electrode catalytic particle electrode.
The catalytic particle electrode is arranged in a three-dimensional electrode reactor with a titanium-based coating electrode as an anode and a graphite electrode as a cathode, and the loading amount is 80%. Under the conditions of 15V voltage, 60min retention time and 90L/h aeration rate, oily sewage with the COD concentration of 1820mg/L is introduced, the COD removal rate after 2h is 80.4 percent, and the COD removal rate after 30h is 78.9 percent.
[ example 4 ]
Grinding 120g of dried gasification furnace slag and 8.4g of sodium carbonate until the mixture is uniformly mixed, placing the mixture in a tubular heating furnace, activating for 4 hours at 500 ℃ in the nitrogen atmosphere, cooling the mixture to room temperature along with the furnace, adding 90mL of 4mol/L hydrochloric acid, soaking for 3 hours, and drying to obtain the modified gasification furnace slag. Taking 70g of modified gasification furnace slag, 15g of clay, 7.5g of ferric oxide and 7.5g of starch, uniformly mixing, adding water to prepare small balls of 30-50mm, drying at 110 ℃ for 2h, roasting the dried small balls in a muffle furnace at 800 ℃ for 4h, and cooling to obtain the three-dimensional electrode catalytic particle electrode.
The catalytic particle electrode is arranged in a three-dimensional electrode reactor with a titanium-based coating electrode as an anode and a graphite electrode as a cathode, and the amount of the device is 60 percent. Under the conditions of 15V voltage, 60min residence time and 90L/h aeration rate, oily sewage with the COD concentration of 1820mg/L is introduced, the COD removal rate after 2h is 71.9 percent, and the COD removal rate after 30h is 70.8 percent.
[ example 5 ]
Grinding 120g of dried gasification furnace slag and 8.4g of sodium carbonate until the mixture is uniformly mixed, placing the mixture in a tubular heating furnace, roasting the mixture for 3 hours at 700 ℃ in the nitrogen atmosphere, cooling the mixture to room temperature along with the furnace, adding 90mL of 3mol/L hydrochloric acid, soaking the mixture for 3 hours, and drying the mixture to obtain the modified gasification furnace slag. Taking 85g of modified gasification furnace slag, 10g of clay, 4g of ferric oxide and 1g of starch, uniformly mixing, adding water to prepare small balls of 30-50mm, drying at 110 ℃ for 2h, roasting the dried small balls in a muffle furnace at 900 ℃ for 2h, and cooling to obtain the three-dimensional electrode catalytic particle electrode.
The catalytic particle electrode is arranged in a three-dimensional electrode reactor with a titanium-based coating electrode as an anode and a graphite electrode as a cathode, and the loading amount is 60%. Under the conditions of 15V voltage, 60min retention time and 90L/h aeration rate, oily sewage with the COD concentration of 1820mg/L is introduced, the COD removal rate after 2h is 88.4 percent, and the COD removal rate after 30h is 86.2 percent.
Comparative example 1
The anode is a titanium-based coating electrode, the cathode is a graphite electrode three-dimensional electrode reactor, and the adsorption saturated columnar activated carbon and ceramsite particle electrode are added into the graphite electrode three-dimensional electrode reactor, wherein the mass ratio of the columnar activated carbon to the ceramsite particles is 8:2. Under the conditions of 15V voltage, 60min retention time and 90L/h aeration rate, oily sewage with the COD concentration of 1820mg/L is introduced, and the COD removal rate is 67.3 percent after 2 h.
Comparative example 2
The anode is a titanium-based coating electrode, the cathode is a graphite electrode, and iron carbon filler and columnar activated carbon which are saturated in adsorption are added into the three-dimensional electrode reactor, wherein the mass ratio of the iron carbon filler to the columnar activated carbon is 8:2. Under the conditions of 15V voltage, 60min retention time and 90L/h aeration rate, oily sewage with the COD concentration of 1820mg/L is introduced, the COD removal rate is 77.7 percent after 2h, iron sludge precipitation appears in the reactor after 30h, and the COD removal rate is reduced to 62.4 percent.
The specific embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (12)
1. A method for preparing a particle electrode is characterized in that gasification furnace slag is used as a raw material, and is subjected to alkali treatment, activation and acid treatment to obtain modified gasification furnace slag, the modified gasification furnace slag is mixed with clay, a foaming agent and a pore-forming agent and is roasted to obtain the particle electrode, and the weight contents of all components are as follows by taking the weight of the particle electrode as a reference: 60-88% of gasifier slag, 10-30% of clay, 1-10% of foaming agent and 1-10% of pore-forming agent.
2. The preparation method according to claim 1, wherein the weight content of each component is as follows: 65-75% of gasifier slag, 15-25% of clay, 3-8% of foaming agent and 3-8% of pore-forming agent.
3. The method according to claim 1, wherein the alkali treatment is mixing and grinding the gasification furnace slag and a carbonate, preferably sodium carbonate or potassium carbonate, until uniform.
4. The preparation method according to claim 3, wherein the mass ratio of the gasification slag to the carbonate is 100 (5-20); preferably, the mass ratio of the gasification slag to the carbonate is 100 (5-10).
5. The method of claim 1, wherein the activation conditions are: the activation temperature is 500-750 ℃, the activation time is 1-4h, and nitrogen is adopted for protection in the activation process; preferably, the activation temperature is 600-700 ℃ and the activation time is 2-3h.
6. The method of claim 1, wherein the acid treatment is: soaking with acid solution with concentration of 2-4mol/L for 2-4h; preferably, the concentration of the acid solution is 2-3mol/L, and the soaking time is 2.5-3.5h.
7. The preparation method according to claim 1, wherein the foaming agent is selected from one or more of iron oxide, magnesium carbonate and silicon carbide; the pore-forming agent is selected from one or more of starch and plant straw.
8. The method of claim 1, wherein the firing conditions are: the roasting temperature is 800-1000 ℃, and the roasting time is 2-4h; preferably, the roasting temperature is 850-950 ℃, and the roasting time is 2-3h.
9. Use of a particle electrode prepared by the method of any one of claims 1 to 8 in a three-dimensional electrode reactor for the treatment of wastewater.
10. The use according to claim 9, wherein the anode of the three-dimensional electrode reactor is a titanium-based coated electrode, the cathode is a graphite electrode, and the filler is the particle electrode according to any one of claims 1 to 8, wherein the loading of the particle electrode is not less than 50%.
11. The use according to claim 9, wherein the three-dimensional electrode reactor is provided with an aeration device which can aerate the inside of the reactor with air, preferably with an aeration rate of 30-150L/h.
12. The use according to claim 9, wherein the operating conditions of the three-dimensional electrode are: the voltage of the three-dimensional electrode reactor is 5-20V, and the retention time is 30-120 min.
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