CN116196725A - Mercury adsorption and adsorbent regeneration device for coal-fired flue gas and mercury removal method - Google Patents
Mercury adsorption and adsorbent regeneration device for coal-fired flue gas and mercury removal method Download PDFInfo
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- CN116196725A CN116196725A CN202310361125.6A CN202310361125A CN116196725A CN 116196725 A CN116196725 A CN 116196725A CN 202310361125 A CN202310361125 A CN 202310361125A CN 116196725 A CN116196725 A CN 116196725A
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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
- B01D53/06—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 moving adsorbents, e.g. rotating beds
- B01D53/10—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 moving adsorbents, e.g. rotating beds with dispersed adsorbents
- B01D53/12—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 moving adsorbents, e.g. rotating beds with dispersed adsorbents according to the "fluidised technique"
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40086—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by using a purge gas
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
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- Treating Waste Gases (AREA)
Abstract
The gas outlet of the adsorbent regeneration fluidized bed is connected with the dust-containing gas inlet of the second cyclone separator through a pipeline, the dust-discharging port of the second cyclone separator is connected with the second adsorbent return port of the adsorbent regeneration fluidized bed through a third material returning device, and the adsorbent outlet of the adsorbent regeneration fluidized bed is connected with the first adsorbent return port of the adsorbent regeneration fluidized bed through a third material returning device; the air inlet of the adsorbent regeneration fluidized bed is communicated with mercury-free nitrogen or air. The invention has high mercury removal efficiency, low mercury removal cost, recycling of mercury removal adsorbent and recycling of flue gas mercury resources.
Description
Technical Field
The invention belongs to the technical field of mercury removal of coal-fired flue gas, and particularly relates to a device and a method for mercury adsorption and adsorbent regeneration of coal-fired flue gas.
Background
Mercury is considered an environmentally highly toxic contaminant due to its strong toxicity, long-range transport, environmental persistence, and bioaccumulation. Coal-fired power plants are one of the main artificial sources of mercury emissions in the environment. In China, the emission concentration limit value of the mercury in the flue gas of the coal-fired power plant is regulated to be 30 mug/m in the emission standard of atmospheric pollutants of the thermal power plant (GB 13223-2011) 3 . Along with the signing of the 'about mercury Water, the convention' predicts that the emission concentration of mercury in flue gas of coal-fired power plants in 2030 needs to reach 3 mug/m 3 The following is given. Therefore, the emission reduction of mercury in flue gas of coal-fired power plants is urgent.
In the prior art, the coal-fired flue gas demercuration mainly adopts the injection demercuration technology with activated carbon as an adsorbent, the device is arranged at the front part of a dust removing device of a coal-fired power plant, the adsorbent is injected into a flue through an injection system, the mercury removal of the adsorbent is realized along with the flow of flue gas, and the adsorbent after mercury removal is collected by a subsequent dust removing device. However, in the operation process of spraying and removing mercury from the adsorbent, if higher mercury removal efficiency is to be achieved, a large amount of mercury removal adsorbent needs to be sprayed, so that the loss of the adsorbent is large, the adsorption efficiency is lower due to the short contact time of the adsorbent and the coal-fired flue gas, and in addition, the adsorbent after mercury removal and the coal-fired fly ash are removed together by the dust removal device. On one hand, the adsorbent has large dosage, cannot be reused and has high use cost; the used adsorbent can have secondary release of mercury and influence the quality of fly ash; on the other hand, the recovery of precious resource mercury can not be realized, which results in large-scale engineering popularization based on the activated carbon injection mercury removal technology.
Disclosure of Invention
The invention solves the defects of the prior art and provides a coal-fired flue gas mercury adsorption and adsorbent regeneration device and a mercury removal method, wherein the device and the method have the advantages of high mercury removal efficiency, low mercury removal cost, recyclable mercury removal adsorbent and capability of recycling flue gas mercury.
In order to achieve the above purpose, the invention firstly provides a coal-fired flue gas mercury adsorption and adsorbent regeneration device, which comprises a demercuration fluidized bed and an adsorbent regeneration fluidized bed, wherein an air inlet of the demercuration fluidized bed is connected with an outlet of an electric dust collector, a first adsorbent inlet of the demercuration fluidized bed is connected with a screw feeding device, demercuration adsorbent is arranged in the demercuration fluidized bed, a gas outlet of the demercuration fluidized bed is connected with a dust-containing gas inlet of a first cyclone separator through a pipeline, a mercury-free gas outlet of the first cyclone separator is connected with an inlet of a wet desulfurization device, a dust discharge port of the first cyclone separator is connected with a second adsorbent inlet of the adsorbent regeneration fluidized bed through a first return device, a gas outlet of the adsorbent regeneration fluidized bed is connected with a dust-containing gas inlet of a second cyclone separator through a pipeline, a high-concentration gas outlet of the second cyclone separator is connected with an inlet of a condensation recovery device, and a dust discharge port of the second cyclone separator is connected with a second adsorbent regeneration fluidized bed through a return device; the air inlet of the adsorbent regeneration fluidized bed is communicated with mercury-free nitrogen or air.
In this embodiment, the gas inlet, the gas outlet, the first adsorbent inlet and the first adsorbent return port of the mercury removal fluidized bed are all provided with valves.
In this embodiment, the gas outlet, the gas inlet, the second adsorbent return port and the adsorbent outlet of the adsorbent regeneration fluidized bed are all provided with valves.
In this embodiment, the mercury-removing adsorbent comprises M having a chemical formula of lattice intercalation and O-S double defects 2 S x -N 2 O y A nanomaterial; wherein M is at least one of Zn, cu and Mo; n is at least one of Fe, mn and Ce; the molar ratio of M to N is 1:1.5-5; the mercury removal adsorbent is used for converting the mercury in the flue gas into the beta-HgS phase product, is favorable for improving the phase purity and stability of the removed product, and can effectively reduce the secondary pollution of the mercury in the flue gas, and of course, the mercury removal adsorbent can also be a renewable mercury removal adsorbent capable of efficiently capturing mercury, such as metal sulfide and sulfur modificationMetal oxides, and the like.
In this embodiment, the temperature in the mercury removal fluidized bed is 100 to 200 ℃, and the temperature in the adsorbent regeneration fluidized bed is 250 to 450 ℃.
In this embodiment, the first cyclone separator and the second cyclone separator adopt cyclone separators with a separation efficiency of greater than 95%.
In this embodiment, the mercury removal adsorbent has a particle size of 0.5 to 1.6mm
The invention also comprises a mercury removal method for the coal-fired flue gas, and the device for adsorbing and regenerating the mercury in the coal-fired flue gas comprises the following steps:
a. delivering the demercuration adsorbent into a distribution plate of a demercuration fluidized bed through a screw feeding device, introducing the coal-fired flue gas discharged by the electric dust collector into the demercuration fluidized bed, and controlling the residence time of the coal-fired flue gas in the demercuration fluidized bed through the control of a valve;
b. separating mercury-free flue gas from an adsorbent through a cyclone separator, and enabling the mercury-free flue gas to enter a subsequent wet desulfurization device;
c. the adsorbent with adsorbed mercury enters an adsorbent regeneration fluidized bed through a first material returning device, nitrogen or air without mercury is introduced into the adsorbent regeneration fluidized bed, the adsorbent with adsorbed mercury is heated and decomposed after being fluidized by the nitrogen or the air, desorption of elemental mercury and regeneration of the adsorbent are realized, gas-solid separation is realized between the regenerated adsorbent and the nitrogen or the air containing high-concentration mercury through a cyclone separator, the nitrogen or the air containing high-concentration mercury enters a condensation recovery device to realize recovery of flue gas mercury, and the regenerated adsorbent enters a distribution plate of the adsorbent regeneration fluidized bed through a second material returning device to realize cyclic regeneration;
d. the regenerated adsorbent enters a demercuration fluidized bed through a third material returning device to realize the recycling of the demercuration adsorbent.
In this embodiment, in step a, the residence time of the mercury removal adsorbent in the mercury removal fluidized bed is controlled by the valve to be 30 to 90 minutes, and the temperature of the mercury removal fluidized bed is 100 to 200 ℃.
In the embodiment, in the step c, the residence time of the adsorbent after adsorbing mercury in the adsorbent regeneration fluidized bed is 30-90 min, the temperature of the regeneration fluidized bed is 250-450 ℃ and the condensation temperature of the condensation recovery device is 0-40 ℃ by controlling a valve.
Compared with the prior art, the invention has the following remarkable advantages:
(1) High mercury removal efficiency and low mercury removal cost:
the invention breaks through the limitation of high adsorbent/mercury ratio in the adsorbent injection mercury removal technology, on one hand, the problem of load increase of the dust remover in the adsorbent injection mercury removal technology is prevented because the device is arranged behind the electric dust remover, meanwhile, the problem of secondary release of mercury in the adsorbent after conventional injection mercury removal is avoided, and the influence of the adsorbent on fly ash quality is prevented.
(2) The on-line synchronous performance of the mercury removal and regeneration of the adsorbent can be realized:
the invention realizes the combination of the demercuration fluidized bed and the adsorbent regeneration fluidized bed through the returning device, the adsorbent regeneration fluidized bed also adopts a gas-solid fluidized bed, the regeneration of the demercuration adsorbent can be realized through the adsorbent regeneration fluidized bed, the regenerated demercuration adsorbent is returned into the demercuration fluidized bed through the returning device, the cost of the adsorbent in demercuration is greatly reduced, the recycling and the recycling of the adsorbent are realized, and simultaneously, the load of a dust remover is reduced, and the secondary release of mercury and the influence on the quality of fly ash are avoided.
(3) And (3) recycling flue gas mercury resources:
according to the invention, when the adsorbent regeneration is realized by the adsorbent regeneration fluidized bed device, the nitrogen or air containing high-concentration mercury can realize the condensation recovery of mercury in the flue gas mercury condensation recovery device, so that the recycling of flue gas mercury is realized.
In conclusion, the invention realizes the purposes of high mercury removal efficiency, low mercury removal cost, recycling of mercury removal adsorbent and recycling of mercury resources in flue gas on the basis of not changing the flue gas pollution control device of the coal-fired power plant, and solves the problem that the conventional adsorbent injection mercury removal technology possibly affects the quality of fly ash and the secondary release of mercury.
Drawings
Fig. 1 is a schematic structural view of the present invention.
FIG. 2 is an SEM image of the materials of example 1, wherein (a) SEM CuS (b) SEM MnO 2 (c)SEM CuS/MnO 2 ；
FIG. 3 is an SEM-EDS image of the mercury removal agent prepared in example 1; according to SEM and SEM-EDS, the composite particles are nano-sized and have certain embedding property between elements.
FIG. 4 is a Hg-TPD chart. The mercury removal product is mainly beta-HgS. The mercury removal product is stable and single.
FIG. 5 is a graph showing mercury removal efficiency of the adsorbents of different cases (examples 1 to 3) within 2 hours.
Fig. 6 is a graph of mercury removal performance for each of the case materials of example 4. And (3) injection: s is S 2 Fe 2 : molar ratio CuS: fe (Fe) 2 O 3 ＝2:2，S 2 Fe 3 : molar ratio CuS: fe (Fe) 2 O 3 ＝2:3，S 2 Fe 4 : molar ratio CuS: fe (Fe) 2 O 3 = 2:4Removal efficiency: mercury removal rate, oxidation rate: oxidation rate, addition rate: adsorption rate.
Fig. 7 is a graph of Hg-TPD of the sorbent mercury removal products of comparative group 1 and experimental group a of example 4.
In the accompanying drawings: 1. electric dust remover; 2. a screw feeder; 3. a mercury removal fluidized bed; 4. a first cyclone separator; 5.a wet desulfurization device; 6. a first return device; 7. regenerating the adsorbent into a fluidized bed; 8. a second cyclone separator; 9. a condensation recovery device; 10. a second material returning device; 11. and a third material returning device.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical solutions of the embodiments of the present invention may be combined with each other, but it is necessary to be based on the fact that those skilled in the art can implement the technical solutions, and when the technical solutions are contradictory or cannot be implemented, the combination of the technical solutions should be considered as not existing, and not falling within the scope of protection claimed by the present invention.
As shown in fig. 1, the invention provides a coal-fired flue gas mercury adsorption and adsorbent regeneration device and a mercury removal method, comprising a mercury removal fluidized bed and an adsorbent regeneration fluidized bed, wherein the bottom of the mercury removal fluidized bed is provided with an air inlet, the top of the mercury removal fluidized bed is provided with an air outlet, a distribution plate is arranged in the mercury removal fluidized bed between the air inlet and the air outlet, a mercury removal adsorbent is arranged on the distribution plate, a first adsorbent inlet and a first adsorbent return opening are arranged on the side wall of the mercury removal fluidized bed and above the distribution plate, and the first adsorbent inlet of the mercury removal fluidized bed is connected with a screw feeding device;
the top of the adsorbent regeneration fluidized bed is provided with a gas outlet, the bottom of the adsorbent regeneration fluidized bed is provided with a gas inlet, a distribution plate is arranged in the adsorbent regeneration fluidized bed and between the gas inlet and the gas outlet, a second adsorbent inlet and a second adsorbent return opening are arranged on the side wall of the adsorbent regeneration fluidized bed and above the distribution plate, an adsorbent outlet is further arranged on the side wall of the adsorbent regeneration fluidized bed, a discharge hole is arranged on the distribution plate, a third return device is arranged below the discharge hole of the distribution plate, and the outlet of the third return device is connected with the first adsorbent return opening of the mercury removal fluidized bed.
The gas outlet of the mercury-removing fluidized bed is connected with the dust-containing gas inlet of the first cyclone separator through a pipeline, the mercury-free gas outlet of the first cyclone separator is connected with the inlet of the wet desulfurization device, the dust discharging port of the first cyclone separator is connected with the second adsorbent inlet of the adsorbent regeneration fluidized bed through a first returning device, the gas outlet of the adsorbent regeneration fluidized bed is connected with the dust-containing gas inlet of the second cyclone separator through a pipeline, the high-concentration mercury-containing gas outlet of the second cyclone separator is connected with the inlet of the condensation recovery device, the dust discharging port of the second cyclone separator is connected with the second adsorbent return port of the adsorbent regeneration fluidized bed through a second returning device, and the adsorbent outlet of the adsorbent regeneration fluidized bed is connected with the first adsorbent return port of the mercury-removing fluidized bed through a third returning device; the air inlet of the adsorbent regeneration fluidized bed is communicated with mercury-free nitrogen or air.
Valves are arranged on the air inlet, the gas outlet, the first adsorbent inlet and the first adsorbent return opening of the demercuration fluidized bed;
and valves are arranged on the gas outlet, the gas inlet, the second adsorbent feed back opening and the adsorbent outlet of the adsorbent regeneration fluidized bed.
By adopting the structure, the device also comprises a mercury removal method for the coal-fired flue gas, and specifically comprises the following steps:
a. delivering the demercuration adsorbent into a distribution plate of a demercuration fluidized bed through a screw feeding device, introducing the coal-fired flue gas discharged by the electric dust collector into the demercuration fluidized bed, and controlling the residence time of the coal-fired flue gas in the demercuration fluidized bed through the control of a valve;
b. separating mercury-free flue gas from an adsorbent through a cyclone separator, and enabling the mercury-free flue gas to enter a subsequent wet desulfurization device;
c. the adsorbent with adsorbed mercury enters an adsorbent regeneration fluidized bed through a first material returning device, nitrogen or air without mercury is introduced into the adsorbent regeneration fluidized bed, the adsorbent with adsorbed mercury is heated and decomposed after being fluidized by the nitrogen or air, desorption of elemental mercury and regeneration of the adsorbent are realized, gas-solid separation is realized between the regenerated adsorbent and the nitrogen or air containing high-concentration mercury through a cyclone separator, the nitrogen or air containing high-concentration mercury enters a condensation recovery device to realize recovery of flue gas mercury, and the separated regenerated adsorbent enters a distribution plate of the adsorbent regeneration fluidized bed through a second material returning device to realize cyclic regeneration;
d. and the regenerated adsorbent in the adsorbent regenerated fluidized bed enters the demercuration fluidized bed through a third material returning device to realize the recycling of the demercuration adsorbent.
In the embodiment, in the step a, the residence time of the mercury removal adsorbent in the mercury removal fluidized bed is 30-90 min under the control of a valve; the temperature of the mercury removal fluidized bed is controlled to be 100-200 ℃.
In the step c, the residence time of the adsorbent after adsorbing mercury in the adsorbent regeneration fluidized bed is 30-90 min under the control of a valve, and the temperature of the regeneration fluidized bed is controlled to be 250-450 ℃; the condensing temperature of the condensing and recycling device is 0 ℃ to-40 ℃ and is optimal (the melting point of mercury is-39 ℃ and the boiling point of mercury is 356.7 ℃ and the mercury is liquid at normal temperature), the condensation of gaseous elemental mercury can be realized below 0 ℃, and the expected condensing recovery rate of the mercury in the flue gas is above 90% at-40 ℃.
The separation efficiency of the first cyclone separator and the second cyclone separator is more than 95%; the adsorption mercury removal efficiency of the mercury removal adsorbent is more than 90%, the particle size of the mercury removal adsorbent in the mercury removal adsorbent is 0.5-1.6 mm, the mercury removal temperature of the adsorbent is 100-200 ℃, and the regeneration temperature of the adsorbent is 250-400 ℃.
The mercury-removing adsorbent in this embodiment is a mercury-removing material comprising M with lattice intercalation and O-S double defects 2 S x -N 2 O y A nanomaterial; wherein M is at least one of Zn, cu and Mo; n is at least one of Fe, mn and Ce; m and N have a molar ratio of 1:1.5-5, x and y are compounds of M and N, respectively, M being the valence of an even number 2 S x 、N 2 O y Can be respectively described as MS x/2 、NO y/2 ，
Preferably, said x and y are compounds of M and N, respectively, M when said valency is even 2 S x 、N 2 O y Can be respectively described as MS x/2 、NO y/2 ；
Preferably, M is Cu and N is Mn. In the invention, the preferable elements can further synergistically improve the mercury removal effect of the worth of material.
Preferably, the molar ratio of M to N is 1:2-4, more preferably 1:2.5-3.5. It was found that, in the preferred proportions, the synergistic effect of the proportions can be further compounded, and the performance can be further synergistically improved.
The preparation method of the mercury removal material comprises the following steps:
will M 2 S x And N 2 O y And carrying out ultrasonic treatment and aging treatment, and then carrying out mechanochemical treatment to obtain the mercury removal material.
In the present embodiment, M 2 S x Can be prepared based on existing means, e.g., as described for M 2 S x Prepared by precipitation of a water-soluble salt of M and an alkali metal sulfide.
In this embodiment, M is 2 S x And N 2 O y The combination of the components and the ultrasonic-mechanical combination is a key to cooperatively construct the special structure and improve the mercury removal capability of the flue gas. According to the invention, through the dual effects of the components and the ultrasonic-mechanical effect, a special mutual embedding structure and a proper active site suitable for gaseous mercury adsorption can be accidentally created, so that the adsorption of the flue gas mercury can be facilitated, the formation of beta-HgS removal products is facilitated, and the adsorption stability of the flue gas mercury is improved.
Preferably, M is 2 S x And N 2 O y Dispersing in the solution and then carrying out ultrasonic treatment;
the ultrasonic power may be adjusted as needed, for example, the ultrasonic power is 50 to 600W, and may be further preferably 100 to 250W in view of the preparation efficiency;
the treatment time of the ultrasound can be controlled as required, for example, when the power is high, the treatment time can be reasonably shortened as required, and when the power is low, the treatment time can be prolonged according to conventional cognition, for example, the treatment time of the ultrasound is 15-120 min, further can be 20-60 min, and still further can be 20-40min.
In this embodiment, the temperature of the aging treatment is, for example, 10 to 50 ℃, and in view of the treatment cost, room temperature may be preferable, and the temperature thereof is, for example, 20 to 35 ℃;
in this embodiment, the aging time is, for example, 1 to 6 hours, and may be further 2 to 4 hours.
Preferably, the mechanochemical treatment is ball milling.
Preferably, the ball material ratio in the ball milling stage=5:1 to 10:1, and the rotation: 100-600rpm/min, revolution: 50-300rpm/min.
In this embodiment, the time of the ball milling stage is, for example, 10 to 60 minutes, and may be further 20 to 40 minutes in view of efficiency and effect.
Preferably, the preparation method of the mercury removal material comprises the following steps:
(1) An amount of metal nitrate [ M (NO) 3 ) x ]With Na and Na 2 S, magnetically stirring to obtain MS x 。
(2) Adding a certain amount of NO to (1) y 。
(3) And (3) carrying out ultrasonic treatment and aging on the mixture in the step (2).
(4) Washing the particles obtained in the step (3) by deionized water, and then centrifugally separating.
(5) And drying the centrifugally separated particles to obtain intermediate product particles.
(6) And (3) treating the intermediate product particles by adopting a mechanochemical method to finally obtain the mercury removal material.
In the invention, M is innovatively formed 2 S x And N 2 O y In combination, the method is further matched with ultrasonic aging-mechanical activation dual reinforcement, so that a lattice mutual embedding interface structure can be constructed, abundant surface active sites are created, the structural stability of components is improved, the adsorption capacity, adsorption stability and regeneration capacity of flue gas mercury are improved, in addition, the method is beneficial to converting the flue gas mercury into beta-HgS with high phase purity, and the problem of secondary pollution commonly existing in the field of flue gas mercury adsorption can be effectively reduced.
The performance of the mercury removal materials was analyzed as follows:
the mercury removal reaction conditions of the adsorbent adopted in the embodiment of the invention are that: adsorption temperature: 150 ℃; total flow of reaction gas: 1L/min of CO 2 Is 12% by volume of O 2 Is 6% by volume, N 2 As a balance gas; and after being mixed in a flue gas preheating and mixing system through a mass flowmeter, all the gases are introduced into a fixed bed adsorption reaction device together. The initial mercury concentration stabilized at 50. Mu.g/m 3 About, the amount of the adsorbent is 0.1g each time, and after the temperature and the mercury concentration of the fixed bed are stable, the bypass is switched to the main path of the adsorption reaction device containing the adsorbent, and an evaluation experiment of the mercury removal of the adsorbent is started.
The mercury removal performance of mechanochemical catalytic enhanced adsorption mercury removal materials was evaluated by the following method 0 Is (Hg) re ) And Hg of 0 Adsorption rate (Hg) ad ) Is defined as follows:
wherein:
hg in flue gas before and after the adsorbent respectively 0 Concentration of [ mu ] g/m 3 The method comprises the steps of carrying out a first treatment on the surface of the m is the total mass mug of mercury in the adsorbent; v is the volume flow of the simulated smoke, 1 multiplied by 10 -3 m 3 And (3) per min, wherein t is the mercury removal time of the adsorbent, and min.
Example 1:
(1) To 100mL of 0.5M [ Cu (NO) 3 ) 2 ]Na is added into the aqueous solution 2 S (Cu/S molar ratio is 1:1), and CuS (M source) is prepared by magnetic stirring.
(2) Adding MnO to (1) 2 (N source, cu/Mn molar ratio 1:3).
(3) And (3) carrying out ultrasonic treatment and aging on the mixed solution in the step (2), wherein the power of ultrasonic treatment is 100W, the time is 30min, the temperature of aging after ultrasonic treatment is 20 ℃, and the time is 3h.
(4) Filtering to separate the particles of the step (3), washing and drying to obtain intermediate product particles.
(5) Carrying out solid-phase ball milling treatment on intermediate product particles, wherein the ball milling conditions are as follows: ball-to-stock ratio = 6-8:1, rotation: 300-350rpm/min, revolution: 200-250rpm/min for 30min, and separating to obtain the mercury-removing material.
The SEM and SEM-EDS of the material are shown in figures 2 and 3, respectively, and have special inter-embedded structures.
Carrying out flue gas mercury adsorption research on the obtained mercury removal material under the conditions, wherein a Hg-TPD diagram of the adsorbed material is shown in fig. 4, and a specific beta-HgS phase is formed; the test results are shown in FIG. 5, and the adsorption effect is close to 100% after the initial and 120 min.
Example 2:
the only difference compared with example 1 is that the amount of adsorbent used was increased 1-fold during the adsorption test, and the other operations and parameters were the same as in example 1, and the adsorption rate is shown in fig. 5. Has excellent adsorption rate (up to 100%) and stability.
Example 3:
the only difference compared to example 1 is that the Cu/Mn molar ratio in (2) was changed, the experimental groups were:
a: the Cu/Mn molar ratio is 1:1, a step of;
b: the Cu/Mn molar ratio is 1:2;
other operations and parameters were the same as in example 1.
The mercury removal efficiency profile of the sorbent over 2 hours is shown in figure 5. The initial adsorption rate of the group A is 80%, and the attenuation is about 45% after 120min of adsorption. The initial adsorption capacity of the group B can reach 99.7%, and 96% of adsorption preservation rate can be obtained after 120min of circulation, so that the group B has good stability.
Example 4
The difference compared with example 1 is only that M and N are changed, in particular that the M source is CuS and the N source is an iron source, in particular Fe 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The experimental groups were:
comparative group 1: only N sources are used, and M sources are not added;
comparative group 2: the molar ratio of Cu/Fe in the M source and the N source is 2:1, a step of;
comparative group 3: the molar ratio of Cu/Fe in the M source and the N source is 2:2;
experiment a group: the molar ratio of Cu/Fe in the M source and the N source is 2:3, a step of;
the experimental results are shown in FIG. 6. It is known that the initial adsorption rate of the experiment A group is 99%; the adsorption rate after 120min was 93%, and an excellent treatment effect was obtained. The Hg-TPD plot of the product obtained in experiment A is shown in FIG. 7, showing the beta-HgS obtained.
Example 5
The difference compared with example 1 is only that M and N are changed, wherein the M source is CuS and the N source is CeO 2 Other operations and parameters were the same as in example 1..
The initial adsorption rate is 98%; the adsorption rate after 120min was 90%.
It is understood from a comparison of examples 1, 4 and 5 that the metal of the present invention can achieve synergy by controlling the process, and good adsorption performance and adsorption stability can be obtained, but better synergy effect can be obtained when M is Cu and N is Mn.
Example 6
The only difference compared to example 1 is that the power of the ultrasound is 200W and the time is 20min. The aging temperature was 30℃and the time was 2 hours. The time of the ball milling stage was 40min.
The adsorption measurement was carried out in the same manner as in example 1, and the adsorption rate at the initial stage and 120min was over 99.5% as in example 1.
Comparative example 1
The only difference compared to example 1 is that M and N are changed, the experimental group is:
a: (2) In the absence of MnO 2 The subsequent ultrasonic-ball milling treatment was performed with a single CuS, and other operations and parameters were the same as in example 1;
b: step 1 is absent, i.e., cuS is not added, and subsequent ultrasonic-ball milling treatment is performed with a single MnO2, and other operations and parameters are the same as in example 1;
c: in the step (1), in order to add copper nitrate and only sodium sulfide, in the step 4, the composite solid of sodium chloride-manganese oxide is obtained by evaporation, and other operations and parameters are the same as in example 1.
D: using CuS and MnS 2 (sulfide of M-N, molar ratio of Cu/Mn same as in example 1);
the measurement was carried out by the method of example 1, and the result was:
a: the initial mercury removal efficiency can reach 100%, and the adsorption rate after 120min is only 52.6%;
the initial mercury removal rate can reach 81.5 percent, and the adsorption rate after 120 minutes is 60.2 percent;
c: the initial mercury removal efficiency can reach 73.6%, and the adsorption rate after 120min is only 49.2%;
d: the initial mercury removal efficiency can reach 100%, and the adsorption rate after 120min is 79.1%;
comparative example 2
The difference compared to example 3 is only that no ultrasonic treatment was performed, but a single ball milling treatment was performed, and in addition, the time of ultrasonic treatment was complemented by ball milling. Other operations and parameters were the same as in example 1.
The results were: the mercury removal efficiency is 94% and the adsorption rate is 92.6%.
Comparative example 3
The only difference compared to example 3 is that no ball milling treatment was performed, but a single ultrasonic treatment was performed, and in addition, the time of ball milling was supplemented by ultrasonic. Other operations and parameters were the same as in example 1.
The results were: the mercury removal efficiency is 92.1% and the adsorption rate is 89.2%.
Therefore, the mercury removal material can realize synergy based on the components and the joint control of the special lattice intercalary hybridization structure among the components, can synergistically improve the removal capacity and the removal efficiency of the mercury in the flue gas, can accidentally convert a mercury removal product into a beta-HgS phase, improves the purity of the product phase, further improves the stability of the mercury removal product, and reduces the secondary pollution problem faced by the gas phase adsorption process. Moreover, the mercury removal material disclosed by the invention has excellent lattice stability and excellent regeneration and repair capability; and the device is matched with the device for use, so that the mercury removal efficiency of the device can be improved.
The foregoing description of the preferred embodiments of the present invention should not be construed as limiting the scope of the invention, but rather utilizing equivalent structural changes made in the present invention description and drawings or directly/indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
1. The utility model provides a fire coal flue gas mercury adsorbs and adsorbent regenerating unit, includes demercuration fluidized bed (3) and adsorbent regeneration fluidized bed (7), its characterized in that: the gas inlet of the demercuration fluidized bed (3) is connected with the outlet of the electric precipitator (1), the first adsorbent inlet of the demercuration fluidized bed (3) is connected with the spiral feeding device (2), the demercuration adsorbent is arranged in the demercuration fluidized bed (3), the gas outlet of the demercuration fluidized bed (3) is connected with the dust-containing gas inlet of the first cyclone separator (4) through a pipeline, the clean gas outlet of the first cyclone separator (4) is connected with the inlet of the wet desulphurization device (5), the dust discharge port of the first cyclone separator (4) is connected with the second adsorbent inlet of the adsorbent regeneration fluidized bed (7) through the first return device (6), the gas outlet of the adsorbent regeneration fluidized bed (7) is connected with the dust-containing gas inlet of the second cyclone separator (8) through a pipeline, the clean gas outlet of the second cyclone separator (8) is connected with the inlet of the condensation recovery device (9), the dust discharge port of the second cyclone separator (8) is connected with the adsorbent regeneration fluidized bed (7) through the second return device (10), and the adsorbent regeneration fluid bed (7) is connected with the adsorbent regeneration port of the third fluidized bed (11); the air inlet of the adsorbent regeneration fluidized bed (7) is communicated with mercury-free nitrogen or air.
2. The coal-fired flue gas mercury adsorption and adsorbent regeneration apparatus of claim 1, wherein: valves are arranged on the air inlet, the gas outlet, the first adsorbent inlet and the first adsorbent return opening of the demercuration fluidized bed (3).
3. The coal-fired flue gas mercury adsorption and adsorbent regeneration apparatus of claim 2, wherein: and valves are arranged on the gas outlet, the gas inlet, the second adsorbent return port and the adsorbent outlet of the adsorbent regeneration fluidized bed (7).
4. A coal combustion flue gas mercury adsorption and adsorbent regeneration apparatus according to any one of claims 1 to 3, wherein: the mercury-removing adsorbent comprises M with chemical formula of lattice intercalation and O-S double defects 2 S x -N 2 O y A nanomaterial; wherein M is at least one of Zn, cu and Mo; n is at least one of Fe, mn and Ce; the molar ratio of M to N is 1:1.5-5.
5. The coal-fired flue gas mercury adsorption and adsorbent regeneration apparatus of claim 4, wherein: the temperature in the mercury removal fluidized bed (3) is 100-200 ℃, and the temperature in the adsorbent regeneration fluidized bed (7) is 250-450 ℃.
6. The coal-fired flue gas mercury adsorption and adsorbent regeneration apparatus of claim 4, wherein: the first cyclone separator (4) and the second cyclone separator (8) adopt cyclone separators with separation efficiency of more than 95 percent.
7. The coal-fired flue gas mercury adsorption and adsorbent regeneration apparatus of claim 4, wherein: the particle size of the mercury removal adsorbent is 0.5-1.6 mm.
8. A method for removing mercury from coal-fired flue gas, which uses the device for adsorbing mercury and regenerating adsorbent in coal-fired flue gas according to claims 4 and 5, and is characterized in that: the method comprises the following steps:
a. delivering the mercury-removing adsorbent into a distribution plate of a mercury-removing fluidized bed (3) through a screw feeding device (2), introducing coal-fired flue gas discharged from an electric dust collector (1) into the mercury-removing fluidized bed (3), and controlling the residence time of the coal-fired flue gas in the mercury-removing fluidized bed (3) through the control of a valve;
b. separating mercury-free flue gas from an adsorbent through a cyclone separator, and enabling the mercury-free flue gas to enter a subsequent wet desulphurization device (5);
c. the adsorbent after adsorbing mercury enters an adsorbent regeneration fluidized bed (7) through a first material returning device (6), nitrogen or air without mercury is introduced into the adsorbent regeneration fluidized bed (7), the adsorbent after adsorbing mercury is heated and decomposed after being fluidized by the nitrogen or the air, desorption of elemental mercury and regeneration of the adsorbent are realized, gas-solid separation is realized between the regenerated adsorbent and the nitrogen or the air containing high-concentration mercury through a cyclone separator, the nitrogen or the air containing high-concentration mercury enters a condensation recovery device (9) to realize recovery of flue gas mercury, and the regenerated adsorbent enters a distribution plate of the adsorbent regeneration fluidized bed (7) through a second material returning device (10) to realize cyclic regeneration;
d. the regenerated adsorbent enters a demercuration fluidized bed (3) through a third material returning device (11) to realize the recycling of the demercuration adsorbent.
9. The method for mercury removal from coal-fired flue gas according to claim 6, wherein: in the step a, the residence time of the mercury removal adsorbent in the mercury removal fluidized bed (3) is 30-90 min under the control of a valve, and the temperature of the mercury removal fluidized bed is 100-200 ℃.
10. The method for mercury removal from coal-fired flue gas according to claim 6, wherein: in the step c, the residence time of the adsorbent after adsorbing mercury in the adsorbent regeneration fluidized bed (7) is 30-90 min under the control of a valve, the temperature of the regeneration fluidized bed is 250-450 ℃, and the condensation temperature of the condensation recovery device (9) is 0-40 ℃.
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