CN112619595A - Attapulgite-based regenerable flue gas demercuration adsorbent and preparation method thereof - Google Patents
Attapulgite-based regenerable flue gas demercuration adsorbent and preparation method thereof Download PDFInfo
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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- 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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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
- B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/25—Coated, impregnated or composite adsorbents
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Abstract
The invention belongs to the technical field of coal-fired flue gas pollutant control, and particularly relates to a renewable flue gas demercuration adsorbent based on attapulgite and a preparation method thereof. The invention utilizes the attapulgite which is a cheap mineral material to prepare the flue gas demercuration adsorbent, effectively utilizes the cheap natural mineral, and has lower cost compared with other types of adsorbents. The flue gas demercuration adsorbent prepared by the invention has magnetism, can be separated and recovered after mercury adsorption is finished, and can be recycled, so that the actual production cost is effectively saved. The flue gas demercuration adsorbent disclosed by the invention is simple in preparation process, environment-friendly and wide in practical application prospect. The flue gas demercuration adsorbent has high demercuration performance, the demercuration efficiency is as high as more than 90%, and the demercuration efficiency is still more than 80% even in sulfur-containing flue gas.
Description
Technical Field
The invention belongs to the technical field of coal-fired flue gas pollutant control, and particularly relates to a renewable flue gas demercuration adsorbent based on attapulgite and a preparation method thereof.
Background
Mercury is a toxic heavy metal element, has volatility, durability and bioaccumulation, can enter a human body through a food chain, and has fatal influence on the nervous system and growth and development of people. The proportion of artificial emissions is highest among all sources of mercury emissions. In artificial emissions, the proportion of coal emissions is the highest.
Three different forms of mercury can be generated in the combustion process of coal, namely bivalent mercury, elementary mercury and granular mercury, wherein the bivalent mercury is easily dissolved in water and can be efficiently removed in a wet desulphurization system, and the granular mercury can be removed together with fly ash in flue gas in the existing ash removal device of a power plant. Compared with bivalent mercury and granular mercury, elemental mercury is difficult to be effectively removed due to high volatility and low water solubility. Many technologies for controlling mercury pollution emission in flue gas generated in coal combustion process are available, and among them, adsorption of mercury in flue gas by adsorbent is the most studied method. The mechanism of adsorption methods relies primarily on porous junctions on the surface of the adsorbent to adsorb contaminants. At present, the mercury removal adsorbent mainly studied comprises activated carbon, fly ash, calcium-based adsorbent, zeolite material and the like. The most studied is the activated carbon adsorbent which has high mercury removal efficiency but high price; the price of the fly ash and the calcium-based adsorbent is low, but the removal efficiency of the elemental mercury is not very high. In addition, the amount of the adsorbent used in the actual industrial production is large, and after mercury removal is completed, the adsorbent is usually mixed with fly ash and cannot be regenerated, so that the operation cost is high. Therefore, finding a new flue gas demercuration adsorbent that is inexpensive, efficient, and regenerable is one of the keys to current work.
Disclosure of Invention
One of the purposes of the invention is to provide a renewable flue gas demercuration adsorbent based on attapulgite, which can effectively remove zero-valent mercury in coal-fired flue gas, and has high demercuration efficiency and good separation cycle regeneration performance.
The invention also aims to provide a preparation method of the renewable flue gas demercuration adsorbent based on attapulgite, which has the advantages of simple preparation process, low cost and easy adjustment.
The scheme adopted by the invention for realizing one of the purposes is as follows: the renewable flue gas demercuration adsorbent is prepared by taking attapulgite as a raw material and utilizing iron oxide magnetic modification and manganese copper nitrate impregnation modification.
The second scheme adopted by the invention for achieving the purpose is as follows: the preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent comprises the following steps:
(1) preparing a ferric salt solution with a certain concentration, adding pretreated attapulgite with a solid-to-liquid ratio of 1: 35-45, uniformly mixing, adding excessive concentrated ammonia water, stirring at a constant temperature to form stable and uniform black turbid liquid, filtering, washing to be neutral, drying, calcining, and grinding to obtain magnetic attapulgite;
(2) and (2) adding a proper amount of the magnetic attapulgite obtained in the step (1) into a manganin salt solution with a certain concentration, soaking, drying and calcining to obtain the regenerable flue gas demercuration adsorbent.
Preferably, in the step (1), the iron salt solution is a mixed salt solution containing iron ions and ferrous ions; the salt containing iron ions is at least one of ferric sulfate, ferric chloride and ferric nitrate; the salt containing ferrous ions is at least one of ferrous sulfate, ferrous chloride and ferrous ammonium sulfate; the mass ratio of the attapulgite to the ferrous ions to the ferric ions is 1: 0.109-0.133: 0.218-0.266.
Preferably, in the step (1), the stirring temperature is 65-75 ℃; the drying temperature is 95-105 ℃.
Preferably, in the step (1), the calcining temperature is 230-270 ℃, and the calcining time is 3-4 h.
Preferably, in the step (1), the attapulgite clay pretreatment step is to add attapulgite clay into water, stir and disperse the attapulgite clay into suspension, and then filter, dry and grind the suspension to obtain the pretreated attapulgite clay.
Preferably, in the step (2), in the manganin salt solution, the manganin salt is at least one of manganese nitrate, manganese chloride and manganese acetate, and the copper salt is at least one of copper nitrate, copper chloride and copper acetate.
Preferably, the mass ratio of the magnetic attapulgite to the manganese ions to the copper ions is 1: 0.08-0.20: 0.013-0.077.
Preferably, in the step (2), the dipping method is ultrasonic dipping, and the drying temperature is 95-105 ℃.
Preferably, in the step (2), the calcining temperature is 400-450 ℃; the calcination time is 3.5-4.5 h.
The material used by the invention is attapulgite which is a layer chain-shaped magnesium-rich silicate clay mineral, is needle-shaped or fibrous, and has larger specific surface area and stronger adsorption performance. The flue gas demercuration adsorbent is prepared from attapulgite serving as a raw material by pretreatment, magnetic modification and active substance loading. The preparation method of the regenerable flue gas demercuration adsorbent is simple and low in cost, can realize separation and recovery and cyclic regeneration and utilization by a simple method besides high demercuration performance, and has high application value and market prospect.
The invention has the following advantages and beneficial effects:
(1) the invention utilizes the attapulgite which is a cheap mineral material to prepare the flue gas demercuration adsorbent, effectively utilizes the cheap natural mineral, and has lower cost compared with other types of adsorbents.
(2) The flue gas demercuration adsorbent prepared by the invention has magnetism, can be separated and recovered after mercury adsorption is finished, and can be recycled, so that the actual production cost is effectively saved.
(3) The flue gas demercuration adsorbent prepared by the invention is simple in preparation process, environment-friendly and wide in practical application prospect.
(4) The flue gas demercuration adsorbent prepared by the invention has higher demercuration performance, the demercuration efficiency is up to more than 90%, and the demercuration efficiency is still more than 80% even in sulfur-containing flue gas.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention for preparing a renewable flue gas demercuration adsorbent based on attapulgite;
fig. 2 is SEM images of raw attapulgite (a) and a renewable flue gas demercuration adsorbent based on attapulgite prepared in the present invention (b), respectively.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1
According to the process flow shown in figure 1, 20g of attapulgite is added into 600ml of deionized water, the mixture is stirred for 45min at normal temperature, the suspension is filtered, the obtained solid is dried in an oven at 100 ℃ for 10h, and then the solid is ground to 80 meshes for later use.
Putting 5g of attapulgite pretreated in the step into 200ml of deionized water, adding 2.14g of ferrous chloride tetrahydrate and 5.83g of ferric chloride hexahydrate, stirring at normal temperature for 30min, adding 30ml of concentrated ammonia water to make the suspension alkaline, heating to 75 ℃, stirring at constant temperature to form stable and uniform black suspension, filtering, washing to be neutral, then placing in a 100 ℃ oven for drying for 12h, and finally placing the obtained solid in a 250 ℃ oven for calcining for 4h to obtain the magnetic attapulgite.
Dispersing 1g of magnetic attapulgite in 10ml of deionized water, adding 0.26g of 50% manganese nitrate solution and 0.076g of copper nitrate, stirring uniformly, ultrasonically soaking for 1.5h, then drying in an oven at 100 ℃ for 12h, then transferring into a muffle furnace, and calcining at 400 ℃ for 4h to obtain the reproducible flue gas demercuration adsorbent. A Scanning Electron Microscope (SEM) of the original attapulgite and a renewable flue gas demercuration adsorbent prepared according to the present invention is shown in fig. 2.
From the comparison of the SEM photographs of the raw attapulgite in fig. 2 with the adsorbent prepared according to the present invention, it was observed that the raw attapulgite had a rod-like structure, and in the adsorbent prepared according to the present invention, crystals having uniform sizes were formed on the surface of the rod-like structure, indicating that both the magnetic substance and the manganese-copper active component were successfully loaded on the surface of the attapulgite.
Example 2
Adding 20g of attapulgite into 600ml of deionized water, stirring at normal temperature for 45min, carrying out suction filtration on the suspension, drying the obtained solid in an oven at 100 ℃ for 10h, and then grinding to 80 meshes for later use.
Putting 5g of attapulgite pretreated in the step into 200ml of deionized water, adding 1.64g of ferrous sulfate monohydrate and 7.84g of ferric nitrate nonahydrate, stirring at normal temperature for 30min, adding 30ml of concentrated ammonia water to make the suspension alkaline, heating to 75 ℃, stirring at constant temperature to form stable and uniform black suspension, filtering, washing to be neutral, then placing in a 100 ℃ oven for drying for 12h, and finally calcining the obtained solid at 250 ℃ for 4h to obtain the magnetic attapulgite.
Dispersing 1g of magnetic attapulgite in 10ml of deionized water, adding 0.39g of 50% manganese nitrate solution and 0.082g of anhydrous copper chloride, stirring uniformly, ultrasonically soaking for 1.5h, drying in a 100 ℃ oven for 12h, transferring into a muffle furnace, and calcining at 400 ℃ for 4h to obtain the reproducible flue gas demercuration adsorbent.
Example 3
Adding 20g of attapulgite into 600ml of deionized water, stirring at normal temperature for 45min, carrying out suction filtration on the suspension, drying the obtained solid in an oven at 100 ℃ for 10h, and then grinding to 80 meshes for later use.
Putting 5g of attapulgite pretreated in the step into 200ml of deionized water, simultaneously adding 4.65g of ammonium ferrous sulfate hexahydrate and 4.73g of ferric sulfate, stirring at normal temperature for 30min, adding 30ml of concentrated ammonia water to make the suspension alkaline, heating to 75 ℃, stirring at constant temperature to form stable and uniform black suspension, filtering, washing to be neutral, then placing in a 100 ℃ oven for drying for 12h, and finally placing the obtained solid at 250 ℃ for calcining for 4h to obtain the magnetic attapulgite.
Dispersing 1g of magnetic attapulgite in 10ml of deionized water, adding 0.183g of anhydrous manganese chloride and 0.19g of copper nitrate, stirring uniformly, ultrasonically soaking for 1.5h, drying in a 100 ℃ oven for 12h, transferring into a muffle furnace, and calcining at 450 ℃ for 4h to obtain the reproducible flue gas demercuration adsorbent.
Example 4
Adding 20g of attapulgite into 600ml of deionized water, stirring at normal temperature for 45min, carrying out suction filtration on the suspension, drying the obtained solid in an oven at 100 ℃ for 10h, and then grinding to 80 meshes for later use.
Putting 5g of attapulgite pretreated in the step into 200ml of deionized water, simultaneously adding 2.14g of ferrous chloride tetrahydrate and 4.32g of ferric sulfate, stirring at normal temperature for 30min, adding 30ml of concentrated ammonia water to make the suspension alkaline, heating to 75 ℃, stirring at constant temperature to form stable and uniform black suspension, filtering, washing to be neutral, then placing in a 100 ℃ oven for drying for 12h, and finally calcining the obtained solid at 250 ℃ for 4h to obtain the magnetic attapulgite.
Dispersing 1g of magnetic attapulgite in 10ml of deionized water, adding 0.356g of manganese acetate tetrahydrate and 0.243g of copper acetate monohydrate, stirring uniformly, ultrasonically soaking for 1.5h, then drying in an oven at 100 ℃ for 12h, then transferring into a muffle furnace, and calcining at 450 ℃ for 4h to obtain the reproducible flue gas demercuration adsorbent.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (10)
1. The utility model provides a flue gas demercuration adsorbent that can regenerate based on attapulgite which characterized in that: the regenerable flue gas demercuration adsorbent is prepared by taking attapulgite as a raw material and utilizing iron oxide magnetic modification and manganese copper nitrate dipping modification.
2. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 1, comprising the steps of:
(1) preparing a ferric salt solution with a certain concentration, adding pretreated attapulgite with a solid-to-liquid ratio of 1: 35-45, uniformly mixing, adding excessive concentrated ammonia water, stirring at a constant temperature to form stable and uniform black turbid liquid, filtering, washing to be neutral, drying, calcining, and grinding to obtain magnetic attapulgite;
(2) and (2) adding a proper amount of the magnetic attapulgite obtained in the step (1) into a manganin salt solution with a certain concentration, soaking, drying and calcining to obtain the regenerable flue gas demercuration adsorbent.
3. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (1), the ferric salt solution is a mixed salt solution containing ferric ions and ferrous ions; the salt containing iron ions is at least one of ferric sulfate, ferric chloride and ferric nitrate; the salt containing ferrous ions is at least one of ferrous sulfate, ferrous chloride and ferrous ammonium sulfate; the mass ratio of the attapulgite to the ferrous ions to the ferric ions is 1: 0.109-0.133: 0.218-0.266.
4. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (1), the stirring temperature is 65-75 ℃; the drying temperature is 95-105 ℃.
5. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (1), the calcining temperature is 230-270 ℃, and the calcining time is 3-4 h.
6. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (1), the step of pre-treating the attapulgite comprises the steps of adding the attapulgite into water, stirring and dispersing the attapulgite into suspension, and then filtering, drying and grinding the suspension to obtain the pre-treated attapulgite.
7. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (2), in the manganin salt solution, the manganese salt is at least one of manganese nitrate, manganese chloride and manganese acetate, and the copper salt is at least one of copper nitrate, copper chloride and copper acetate.
8. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (2), the mass ratio of the magnetic attapulgite to the manganese ions to the copper ions is 1: 0.08-0.20: 0.013-0.077.
9. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (2), the dipping method is ultrasonic dipping, and the drying temperature is 95-105 ℃.
10. The preparation method of the attapulgite-based regenerable flue gas demercuration adsorbent according to claim 2, wherein: in the step (2), the calcining temperature is 400-450 ℃; the calcination time is 3.5-4.5 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114259978A (en) * | 2021-12-27 | 2022-04-01 | 杭州电子科技大学 | Preparation process of efficient coal-fired flue gas demercuration adsorbent and product thereof |
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Application publication date: 20210409 |