CN114452935A - Method for preparing carbon-based denitration efficient adsorbent by using short chain - Google Patents
Method for preparing carbon-based denitration efficient adsorbent by using short chain Download PDFInfo
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- CN114452935A CN114452935A CN202210140668.0A CN202210140668A CN114452935A CN 114452935 A CN114452935 A CN 114452935A CN 202210140668 A CN202210140668 A CN 202210140668A CN 114452935 A CN114452935 A CN 114452935A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
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- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
Abstract
The invention discloses a method for preparing a carbon-based denitration efficient adsorbent by using a short chain, and belongs to the field of preparation and denitration of activated carbon. The method comprises the steps of taking east China raw coal as a raw material, processing the raw material through the processes of crushing, acidification, suction filtration, drying, carbonization and the like to obtain a carbonized carbon material, and then carrying out the processes of dipping, activating, roasting and the like on the carbon material to obtain the efficient adsorbent. The invention relates to a method for preparing a carbon-based denitration efficient adsorbent by using a short chain, which aims to achieve a good adsorption denitration effect under the condition that only one chemical reagent is added without loading a metal element through a series of process flows and has the characteristics of simple preparation method, short period, economy, environmental protection and the like.
Description
Technical Field
The invention relates to the technical field of preparation and denitration of activated carbon, in particular to a method for preparing a carbon-based denitration efficient adsorbent by using a short chain.
Background
Along with the continuous deepening of enterprise renovation and rural scattered coal treatment work, the demand of clothes, eating and housing people for electricity is larger and larger, the scale of a coal-fired power plant needs to be enlarged continuously, and the harmful pollutants discharged by the coal-fired power plant are increased in proportion, wherein nitrogen oxides not only can cause acid rain and photochemical smog, but also can cause respiratory system diseases, and can cause cancers in severe cases.
Activated carbon is often used as an adsorbent to purify atmospheric pollutants due to its loose porous nature and good adsorption properties. The activated carbon prepared in the Chinese patent CN 108246095A is soaked by alkali liquor, then is irradiated by microwaves, is adjusted to be neutral by acid washing, enables the steel slag micro powder to be reused, and carries out flue gas denitration by taking metal oxide in the steel slag micro powder as a catalyst and taking C and CO in the activated carbon as reducing agents.
Not only NO present in the flue gasxAlso in the presence of SO2Pollutant such as dust, vapor at the in-process of denitration, SO 2's existence can lead to the competition to adsorb for denitration effect variation, and on the other hand, when having metallic element in the catalyst, can make the denitration efficiency of catalyst improve greatly, nevertheless simultaneously because SO is because the denitration efficiency of catalyst improves greatly2The presence of (2) can generate sulfate precipitates which adhere to the surface of the catalyst and cause catalyst poisoning, and therefore, the sulfur resistance of the adsorbent in the form of a composite of the metal oxide and the carbon-based material is poor. The carbon-based adsorbent is activated by adopting trace alkaline metal or carbon-based material, the preparation is simple, and the adsorption volume of the nitrogen oxide of the prepared catalyst is greatly improved.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a method for preparing a carbon-based denitration efficient adsorbent by using a short chain, which has the advantages of reasonable structure, strong practicability and good using effect.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for preparing a carbon-based denitration efficient adsorbent by using a short chain is characterized by comprising the following steps:
(1) pretreatment of
Cleaning and drying east raw coal, then crushing, and screening to obtain target powder;
(2) acidification demineralization
Putting the pretreated powder into a mixed solution of nitric acid and hydrochloric acid, heating in a water bath, cooling, performing suction filtration, and drying to obtain treated raw coal powder;
(3) preliminary carbonization
Calcining the treated raw coal powder in a tubular furnace in a nitrogen atmosphere to obtain a primarily carbonized carbon material;
(4) hydrothermal reaction
Will K2CO3Mixing the solution and the preliminarily carbonized carbon material, putting the mixture into a hydrothermal reaction kettle, putting the reaction kettle into a drying box for hydrothermal reaction, cooling, and drying the carbon material;
(5) calcination and further activation
And calcining the carbon material obtained in the last step in a nitrogen and carbon dioxide atmosphere by using a tube furnace, further activating the carbon material, and then cooling the carbon material to room temperature in a protective nitrogen atmosphere to obtain the carbon-based adsorbent.
Further, in the step 1, cleaning is carried out to remove miscellaneous ores and humus contained in the coal, and the crushed particle size of the raw coal in the east China is 30-50 meshes.
Further, the ratio of nitric acid to hydrochloric acid in the acid solution prepared by acid washing in the step 2 is 2: 1.
further, in the acid washing process in the step 2, the beaker is sealed, the heating temperature is 60-90 ℃, the temperature is kept for 2-12h, and the deionized water is adopted for suction filtration after cooling to ensure that the residual acidic substances on the surface of the carbon material are washed away.
Further, the carbon material after suction filtration in the step 2 is dried for 2-24h at the temperature of 100-120 ℃ by using an air drying oven, and is preferably dried for 4h at the temperature of 105 ℃.
Further, in the step 3, the heating temperature of the tubular furnace is 400-.
Further, K in the step 42CO3The concentration of the solution is 0.1mol/L, the temperature of the reaction kettle is 120-200 ℃, and the heat preservation time is 12-48 h.
Further, after the hydrothermal reaction in the step 4 is finished, cooling the reaction product by adopting a step cooling method.
Further, the temperature during the calcination in the step 5 is 700-1000 ℃, and the temperature is kept for 1-5 h.
Further, when the temperature is increased to the specified calcination in the step 5, CO is introduced2Stopping introducing CO after the heat preservation is finished2(ii) a The flow rate of the gas introduced in the step 5 is 1000ml/min, wherein CO is2And N2In a ratio of 1: 4.
Compared with the prior art, the invention has the advantages that:
(1) the method for preparing the catalyst is simple, and only K is added in the activation process2CO3A chemical reagent has short production period, can achieve excellent adsorption denitration effect, and reduces the generation of harmful gas.
(2) The raw coal is used as a precursor, the material is easy to obtain, the cost is low, and the preparation process does not influence the environment.
(3) The catalyst can be recycled through in-situ regeneration treatment, so that the cost is reduced.
Drawings
FIG. 1 is a graph showing the adsorption curves of the adsorbents obtained by the present invention at different calcination temperatures.
Fig. 2 is a scanning electron microscope image of the resulting adsorbent calcined at 700 ℃.
FIG. 3 is a scanning electron micrograph of the resulting sorbent calcined at 800 ℃.
Fig. 4 is a scanning electron microscope image of the resulting adsorbent calcined at 900 ℃.
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings. In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
(1) the eastern Junggar raw coal is cleaned, dried, crushed and sieved to obtain 30-50 mesh powder.
(2) And (3) putting the pretreated powder into a mixed solution of nitric acid and hydrochloric acid in a ratio of 2:1, heating the mixed solution to 80 ℃ in a water bath, preserving the heat for 2 hours, cooling, performing suction filtration, and drying to obtain the treated raw coal powder.
(3) And calcining the treated raw coal powder in a tubular furnace at 600 ℃ for 2h under the nitrogen atmosphere at the heating rate of 10 ℃/min to obtain the primarily carbonized carbon material.
(4) K is prepared in 0.1mol/L2CO3And mixing the solution with the preliminarily carbonized carbon material, putting the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, controlling the temperature at 160 ℃, keeping the temperature for 24 hours to perform hydrothermal reaction, cooling, and drying the carbon material.
(5) Heating the carbon material obtained in the previous step to 700 ℃ in a tubular furnace under nitrogen atmosphere, and then introducing carbon dioxide at a gas flow rate of 1000ml/min, wherein the CO is2And N2The ratio of the components is 1:4, the temperature is kept for 2h, and the carbon-based adsorbent is obtained after the carbon-based adsorbent is cooled to room temperature in the protective nitrogen atmosphere.
Example 2:
(1) the eastern Junggar raw coal is cleaned, dried, crushed and sieved to obtain 30-50 mesh powder.
(2) And (3) putting the pretreated powder into a mixed solution of nitric acid and hydrochloric acid in a ratio of 2:1, heating the mixed solution to 80 ℃ in a water bath, preserving the heat for 2 hours, cooling, performing suction filtration, and drying to obtain the treated raw coal powder.
(3) And calcining the treated raw coal powder in a tubular furnace at 600 ℃ for 2h under the nitrogen atmosphere at the heating rate of 10 ℃/min to obtain the primarily carbonized carbon material.
(4) K is prepared in 0.1mol/L2CO3And mixing the solution with the preliminarily carbonized carbon material, putting the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, controlling the temperature at 160 ℃, keeping the temperature for 24 hours to perform hydrothermal reaction, cooling, and drying the carbon material.
(5) Heating the carbon material obtained in the previous step to 800 ℃ in a tubular furnace under nitrogen atmosphere, and then introducing carbon dioxide at a gas flow rate of 1000ml/min, wherein the CO is2And N2The ratio of the components is 1:4, the temperature is kept for 2h, and the carbon-based adsorbent is obtained after the carbon-based adsorbent is cooled to room temperature in the protective nitrogen atmosphere.
Example 3:
(1) the eastern Junggar raw coal is cleaned, dried, crushed and sieved to obtain 30-50 mesh powder.
(2) And (3) putting the pretreated powder into a mixed solution of nitric acid and hydrochloric acid in a ratio of 2:1, heating the mixed solution to 80 ℃ in a water bath, preserving the heat for 2 hours, cooling, performing suction filtration, and drying to obtain the treated raw coal powder.
(3) And calcining the treated raw coal powder in a tubular furnace at 600 ℃ for 2h under the nitrogen atmosphere at the heating rate of 10 ℃/min to obtain the primarily carbonized carbon material.
(4) K is prepared in 0.1mol/L2CO3And mixing the solution with the preliminarily carbonized carbon material, putting the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, controlling the temperature at 160 ℃, keeping the temperature for 24 hours to perform hydrothermal reaction, cooling, and drying the carbon material.
(5) Heating the carbon material obtained in the previous step to 900 ℃ in a tubular furnace under nitrogen atmosphere, and then introducing carbon dioxide at a gas flow rate of 1000ml/min, wherein the CO is2And N2The ratio of the components is 1:4, the temperature is kept for 2h, and the carbon-based adsorbent is obtained after the carbon-based adsorbent is cooled to room temperature in the protective nitrogen atmosphere.
In order to better reveal the adsorption performance of the adsorbent on VOCs, ethyl acetate, which is a typical VOCs, is selected as the adsorbate. Where C0 is the inlet ethyl acetate concentration (ppm) and C is the outlet concentration (ppm), FIG. 1 shows the adsorption energy for ethyl acetate for these three adsorbents. As can be seen from the adsorption dynamic graph, the breakthrough time is longest when the calcination temperature is 800 ℃ compared with the adsorption effect of the catalysts prepared at the other two calcination temperatures, which indicates that the preparation effect of the adsorbent is the best at the calcination temperature.
The present invention and the embodiments thereof have been described above, and the description is not restrictive, and the embodiments shown in the detailed description are only a part of the embodiments of the present invention, not all embodiments, and the actual configuration is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing a carbon-based denitration efficient adsorbent by using a short chain is characterized by comprising the following steps:
(1) pretreatment of
Cleaning and drying east raw coal, then crushing, and screening to obtain target powder;
(2) acidification demineralization
Putting the pretreated powder into a mixed solution of nitric acid and hydrochloric acid, heating in a water bath, cooling, performing suction filtration, and drying to obtain treated raw coal powder;
(3) preliminary carbonization
Calcining the treated raw coal powder in a tubular furnace in a nitrogen atmosphere to obtain a primarily carbonized carbon material;
(4) hydrothermal reaction
Will K2CO3Mixing the solution and the preliminarily carbonized carbon material, putting the mixture into a hydrothermal reaction kettle, putting the reaction kettle into a drying box for hydrothermal reaction, cooling, and drying the carbon material;
(5) calcination and further activation
And calcining the carbon material obtained in the last step in a nitrogen and carbon dioxide atmosphere by using a tube furnace, further activating the carbon material, and then cooling the carbon material to room temperature in a protective nitrogen atmosphere to obtain the carbon-based adsorbent.
2. The method for preparing the carbon-based denitration efficient adsorbent by the short chain according to claim 1, wherein the cleaning in the step 1 is carried out to remove the miscellaneous minerals and humus contained in the coal, and the crushed particle size of the eastern Junggar raw coal is 30-50 meshes.
3. The method for preparing the carbon-based denitration efficient adsorbent by using the short chain according to claim 1, wherein the ratio of nitric acid to hydrochloric acid in the acid solution prepared by acid washing in the step 2 is 2: 1.
4. the method for preparing the carbon-based denitration high-efficiency adsorbent by using the short chain as claimed in claim 1, wherein in the acid washing process in the step 2, the beaker is sealed, the heating temperature is 60-90 ℃, the temperature is kept for 2-12h, and the acid substances remained on the surface of the carbon material are washed away by suction filtration by using deionized water after cooling.
5. The method for preparing the carbon-based denitration efficient adsorbent by the short chain as claimed in claim 1, wherein the carbon material after suction filtration in the step 2 is dried at 120 ℃ for 2-24h, preferably at 105 ℃ for 4h by using a forced air drying oven.
6. The method for preparing the carbon-based denitration high-efficiency adsorbent by the short chain as claimed in claim 1, wherein the heating temperature of the tubular furnace in the step 3 is 400-.
7. The method for preparing the carbon-based denitration efficient adsorbent by using the short chain as claimed in claim 1, wherein K in the step 42CO3The concentration of the solution is 0.1mol/L, the temperature of the reaction kettle is 120-200 ℃, and the heat preservation time is 12-48 h.
8. The method for preparing the carbon-based denitration efficient adsorbent by the short chain according to claim 1, wherein the hydrothermal reaction in the step 4 is finished, and the carbon-based denitration efficient adsorbent is cooled by a rapid cooling method.
9. The method for preparing the carbon-based denitration efficient adsorbent by the short chain as claimed in claim 1, wherein the calcination temperature in the step 5 is 700-1000 ℃, and the temperature is maintained for 1-5 h.
10. The method for preparing the carbon-based denitration efficient adsorbent by using the short chain as claimed in claim 1, wherein when the calcination temperature in the step 5 is raised to a specified calcination temperature, CO is introduced2Stopping introducing CO after the heat preservation is finished2(ii) a The flow rate of the gas introduced in the step 5 is 1000ml/min, wherein CO is2And N2In a ratio of 1: 4.
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|---|---|---|---|---|
| TWI272248B (en) * | 2002-04-19 | 2007-02-01 | King Car Food Ind Co Ltd | Method for manufacturing activated carbon from coffee waste |
| JP2014129200A (en) * | 2012-12-28 | 2014-07-10 | Kansai Coke & Chem Co Ltd | Active carbon and manufacturing method thereof |
| CN105688806A (en) * | 2016-01-08 | 2016-06-22 | 中国环境科学研究院 | Method for preparing mesoporous carbon from municipal sewage plant sludge in thermal activation mode and sludge-based mesoporous carbon material |
| CN109835900A (en) * | 2019-03-21 | 2019-06-04 | 哈尔滨工业大学 | A kind of preparation method of the coal base porous carbon based on potassium carbonate cyclic activation and the preparation method of biomass-based porous carbon |
| CN110681238A (en) * | 2019-10-24 | 2020-01-14 | 华北电力大学（保定） | New process for treating VOCs (volatile organic compounds) by modified fly ash |
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-
2022
- 2022-02-16 CN CN202210140668.0A patent/CN114452935A/en active Pending
Patent Citations (7)
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| TWI272248B (en) * | 2002-04-19 | 2007-02-01 | King Car Food Ind Co Ltd | Method for manufacturing activated carbon from coffee waste |
| JP2014129200A (en) * | 2012-12-28 | 2014-07-10 | Kansai Coke & Chem Co Ltd | Active carbon and manufacturing method thereof |
| CN105688806A (en) * | 2016-01-08 | 2016-06-22 | 中国环境科学研究院 | Method for preparing mesoporous carbon from municipal sewage plant sludge in thermal activation mode and sludge-based mesoporous carbon material |
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| CN110681238A (en) * | 2019-10-24 | 2020-01-14 | 华北电力大学（保定） | New process for treating VOCs (volatile organic compounds) by modified fly ash |
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| CN112645323A (en) * | 2020-11-24 | 2021-04-13 | 西南科技大学 | Preparation method of cocklebur fruit shell based biomass charcoal adsorbent and application of cocklebur fruit shell based biomass charcoal adsorbent in adsorption of radioactive radon gas |
Non-Patent Citations (1)
| Title |
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| JIN CHUNJIANG: "Adsorption and Regeneration of Volatile Organic Compounds (VOCs) on Coal-Based Activated Carbon by Ferric Nitrate Modification", 《CHINA PETROLEUM PROCESSING AND PETROCHEMICAL TECHNOLOGY》 * |
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Application publication date: 20220510 |