CN114632406B - Preparation method and device of supported carbon dioxide solid adsorbent - Google Patents

Preparation method and device of supported carbon dioxide solid adsorbent Download PDF

Info

Publication number
CN114632406B
CN114632406B CN202210190647.XA CN202210190647A CN114632406B CN 114632406 B CN114632406 B CN 114632406B CN 202210190647 A CN202210190647 A CN 202210190647A CN 114632406 B CN114632406 B CN 114632406B
Authority
CN
China
Prior art keywords
active component
fluidized bed
carbon dioxide
porous carrier
bed body
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210190647.XA
Other languages
Chinese (zh)
Other versions
CN114632406A (en
Inventor
马吉亮
智远
陈晓平
刘道银
鲍学兵
潘苏阳
梁财
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Southeast University
Original Assignee
Southeast University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Southeast University filed Critical Southeast University
Priority to CN202210190647.XA priority Critical patent/CN114632406B/en
Publication of CN114632406A publication Critical patent/CN114632406A/en
Application granted granted Critical
Publication of CN114632406B publication Critical patent/CN114632406B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
    • 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
    • B01D53/81—Solid phase processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/30—Alkali metal compounds
    • B01D2251/304—Alkali metal compounds of sodium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/30—Alkali metal compounds
    • B01D2251/306—Alkali metal compounds of potassium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/60—Inorganic bases or salts
    • B01D2251/606—Carbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention relates to a preparation method of a supported carbon dioxide solid adsorbent, which comprises the following steps: high-temperature air is used as a fluidizing medium to lead the porous carrier particles to be circularly fluidized in the fluidized bed; spraying the active component solution into the fluidized bed from the bottom of the bed after atomization, and immersing atomized liquid drops into porous carrier particle pore channels; simultaneously using high-temperature air as a drying medium to evaporate active component droplets immersed in the porous carrier pore channel, wherein the active component is loaded on the pore channel wall surface of the porous carrier particles; the completed loaded particles are calcined. The preparation device comprises a fluidized bed body, wherein a flow guide pipe is arranged in the fluidized bed body, the flow guide pipe is coaxially arranged with the central shaft of the fluidized bed body and is close to an air distribution plate at the bottom of the fluidized bed body, and the flow guide pipe is used for guiding the fluidization direction of the porous carrier particles. The invention aims to ensure that carbon dioxide and active components react more fully in the diffusion process in the pore channel, thereby improving the adsorption quantity and reducing the energy consumption.

Description

Preparation method and device of supported carbon dioxide solid adsorbent
Technical Field
The invention relates to the technical field of solid adsorbent preparation, in particular to a preparation method and a device of a supported carbon dioxide solid adsorbent.
Background
At present, typical CO 2 The trapping technique includes a chemical absorption method (MEA method, hot potash method, etc.), a membrane separation method, and a solid adsorption method. Among them, the solid adsorption method represented by the alkali metal-based adsorbent has the advantages of low energy consumption, high thermal stability, no corrosion, no secondary pollution, and the like. CO based on alkali metal based sorbents 2 The solid adsorption method is to load an active component (potassium carbonate or sodium carbonate) in the internal pore channels of a porous carrier to prepare the solid adsorbent. In the capture process, the adsorbent reacts CO by adsorption 2 Is captured from the flue gas with complex components and then releases high-purity CO through regeneration reaction 2 And simultaneously, the regeneration of the adsorbent is completed. The core of the technology lies in the preparation ofHigh adsorption capacity, high strength, high activity and low energy consumption.
There are two conventional methods for preparing an alkali metal-based solid adsorbent. One is a solution equal-volume impregnation method, namely, according to the pore volume of a porous carrier, preparing an active component into a solution with the equal volume, then soaking the porous carrier into the solution, and after the carrier completely absorbs the active component solution, drying and calcining to prepare the adsorbent. Research related to the technology is carried out by the university of southeast, and a high-activity sodium-based solid carbon dioxide adsorbent (publication number CN 103480273A) is prepared. The preparation method of the adsorbent has a limited amount of active component supported on a unit mass of the carrier, since the volume of the active component solution is equal to the pore volume of the carrier and the solubility of the solution is fixed at a certain temperature. The other method is a powder forming method, namely, carrier powder and active component solution are mixed and dried, so that the active component is loaded on the surface of the carrier powder. The powder is then bound into large size particles and finally calcined into the sorbent. The relevant literature includes: chang Minghua, chen Xiaoping, cai Tianyi, et al 2 Influence of adsorption Property [ j]Chinese electro-mechanical engineering newspaper (nature science edition), 2021, 41 (11): 3683-3692. And a preparation method of the high-efficiency sodium-based solid decarbonization adsorbent applied to southeast university (with the publication number of CN 108514861A).
The defects of the traditional preparation method are as follows: and (1) the active component is uniformly loaded in the carrier. Due to the short residence time of the adsorbent in the reactor and the CO 2 Diffusion resistance exists in the diffusion inside the pore channel, so that the active component is difficult to be completely mixed with CO 2 Reaction, the adsorbent adsorption capacity is low, and the energy consumption is high; (2) The combination of crystal nuclei occurs during the drying process of the active component solution, which results in larger crystal size on the carrier and smaller effective exposed surface, and also results in reduced adsorption capacity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and a device of a supported carbon dioxide solid adsorbent, which adopt the technical scheme of preparing the adsorbent based on fluidized bed spray impregnationThe purpose is to solve the problem of alkali metal-based CO 2 The active component loading depth, the crystallization size and the appearance are uncontrollable in the preparation process of the solid adsorbent.
The technical scheme adopted by the invention is as follows:
in one aspect, the present application provides a method for preparing a supported carbon dioxide solid adsorbent, comprising:
high-temperature air is used as a fluidizing medium to ensure that the porous carrier particles are circularly fluidized in the fluidized bed;
spraying the active component solution into the fluidized bed from the bottom of the bed after atomization, and immersing atomized liquid drops into porous carrier particle pore channels;
the high-temperature air is simultaneously used as a drying medium, so that active component liquid drops immersed into the pore channels of the porous carrier are evaporated, and the active components are loaded on the wall surfaces of the pore channels of the porous carrier particles;
and calcining the loaded particles to obtain the loaded carbon dioxide solid adsorbent.
The further technical scheme is as follows:
the active ingredient solution is atomized and then continuously or intermittently sprayed into the fluidized bed.
The porous carrier particles are Y-type alumina; the active component solution is a mixed solution of sodium carbonate and potassium carbonate.
In the preparation process, the temperature of the fluidized bed is controlled within 20-70 ℃, the velocity of the fluidized medium is controlled within 0.95-3.87 m/s, and the loading time of the active component solution is controlled within 90-250 min.
Prior to loading, the porous support particles were placed in a drying oven to be completely dried and cooled.
On the other hand, the application provides a preparation device of a loaded carbon dioxide solid adsorbent, which comprises a fluidized bed body, wherein a flow guide pipe is arranged in the fluidized bed body, is coaxially arranged with the central axis of the fluidized bed body and is close to an air distribution plate at the bottom of the fluidized bed body, and is used for guiding the fluidization direction of porous carrier particles;
the double-fluid nozzle penetrates through the air distribution plate and is aligned with the lower end opening of the flow guide pipe; the two-fluid nozzle is for ejecting atomized droplets of the active component.
The further technical scheme is as follows:
the double-fluid nozzle is simultaneously connected with high-pressure air and active component solution through a pipeline, and an air pressure regulating valve and a solution flow control device are arranged on the pipeline.
And a bag-type dust collector is arranged at the top of the fluidized bed body.
The invention has the following beneficial effects:
(1) The evaporation rate of the active component liquid drops in the inner part of the pore channels of the carrier can be controlled by adjusting the drying strength, and further the loading depth of the active component liquid drops in the inner part of the pore channels can be controlled. The carbon dioxide can be more fully reacted with the active component in the diffusion process in the pore channel in the adsorption process, thereby improving the adsorption quantity and reducing the energy consumption.
(2) The invention atomizes the active component solution into small drops which are respectively immersed into the carrier pore channels, thereby weakening the phenomenon of crystal nucleus combination in the solution evaporation process. Compared with the traditional equivoluminal solution impregnation method, the method has the advantages that the number of crystals on the carrier is obviously increased, the effective exposure area is increased, and the adsorption quantity of the adsorbent is further improved.
(3) Compared with the traditional solution impregnation method, the method is not limited by solubility, and can load more active components on the carrier in unit mass, thereby improving the adsorption capacity of the adsorbent.
Drawings
Fig. 1 is a schematic structural diagram of a manufacturing apparatus according to an embodiment of the present invention.
In the figure: 1. a bag-type dust collector; 2. a circular cylinder; 3. porous carrier particles; 4. a tapered barrel; 5. a flow guide pipe; 6. a wind distribution plate; 7. a two-fluid nozzle; 8. a thermometer; 9. an air filter; 10. an electric heater; 11. an air chamber; 12. a storage tank; 13. a peristaltic pump; 14. an air compressor; 15. a pressure regulating valve; 16. a flow meter; 17. an induced draft fan.
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
The preparation method of the supported carbon dioxide solid adsorbent comprises the following steps:
high-temperature air is used as a fluidizing medium to lead the porous carrier particles to be circularly fluidized in the fluidized bed;
spraying the active component solution into the fluidized bed from the bottom of the bed after atomization, and immersing atomized liquid drops into porous carrier particle pore channels; simultaneously using high-temperature air as a drying medium to evaporate active component droplets immersed in the porous carrier pore channel, wherein the active component is loaded on the pore channel wall surface of the porous carrier particles;
and calcining the loaded particles to obtain the loaded carbon dioxide solid adsorbent.
The preparation method further comprises the following steps:
before loading, placing the porous carrier particles in a drying oven for complete drying and cooling;
preparing an active component solution by using deionized water;
the active ingredient solution is atomized and then continuously or intermittently sprayed into the fluidized bed.
Specifically, the porous carrier particles are Y-type alumina with developed pore structure; the active component solution is a mixed solution of sodium carbonate and potassium carbonate.
Specifically, in the preparation process, the temperature of the fluidized bed is controlled within 20-70 ℃, the speed of the fluidized medium is controlled within 0.95-3.87 m/s, and the loading time of the active component solution is controlled within 90-250 min. The numerical ranges include the numerical values of the nodes.
According to the preparation method, the active component solution is atomized and sprayed into the fluidized bed to be mixed with the carrier particles in a fluidized state. The high-temperature air is used as fluidizing air (fluidizing medium) to make the carrier particles in a circulating fluidized state and also used as a drying medium to evaporate water in the active component droplets and make the active components smoothly loaded on the wall surfaces of the porous carrier particle pore passages.
According to the preparation method, the evaporation rate of active component liquid drops in the carrier pore channel and on the particle surface can be controlled by adjusting the drying strength including the parameters of the fluidization wind speed, the temperature of the fluidized bed, the loading time of the active component solution and the like according to actual needs, and further the loading depth of the active component liquid drops in the pore channel is controlled.
Wherein the specific setting of the loading time is determined by the solution mass and the liquid injection flow rate.
According to the preparation method, the processes of impregnation loading and drying in the carrier pore channel are completed simultaneously after the active component solution is atomized, so that the preparation method is not limited by the solubility, more active components can be loaded on the carrier with unit mass, and the adsorption capacity of the adsorbent is improved.
The preparation device of the loaded carbon dioxide solid adsorbent comprises a fluidized bed body, wherein a flow guide pipe is arranged in the fluidized bed body, the flow guide pipe is coaxially arranged with the central shaft of the fluidized bed body and is close to an air distribution plate at the bottom of the fluidized bed body, and the flow guide pipe is used for guiding the fluidization direction of porous carrier particles;
the double-fluid nozzle penetrates through the air distribution plate and is aligned with the lower end opening of the flow guide pipe; the two-fluid nozzle is for ejecting atomized droplets of the active component.
Specifically, the two-fluid nozzle is simultaneously connected with high-pressure air and active component solution through a pipeline, and an air pressure regulating valve and a solution flow control device are arranged on the pipeline.
Specifically, a bag-type dust collector is arranged at the top of the fluidized bed body.
In one embodiment, the present application relates to a device for preparing a supported carbon dioxide solid adsorbent, which can refer to fig. 1, and comprises a conical cylinder 4 as a fluidized bed body, wherein a flow guide pipe 5 is arranged inside the conical cylinder, the flow guide pipe 5 is arranged coaxially with the central axis of the fluidized bed body and is close to a wind distribution plate 6 at the bottom of the fluidized bed body, and the flow guide pipe 5 is used for guiding the fluidization direction of the porous carrier particles 3, so that the porous carrier particles 3 move from the inside of the flow guide pipe 5 to the inside of the conical cylinder 4 of the fluidized bed outside the flow guide pipe 5 from bottom to top in the fluidized bed, and then enter from the bottom of the flow guide pipe 5 to form a directional circulating flow, thereby promoting the directional circulation of the particles. The direction of the circulating flow is indicated by the arrows in fig. 1.
The double-fluid nozzle 7 penetrates through the air distribution plate 6 and is aligned with the lower end opening of the guide pipe 5; the two-fluid nozzle 7 is used to eject atomized droplets of the active component.
Specifically, the two-fluid nozzle 7 is simultaneously connected with high-pressure air and active component solution through a pipeline, and an air pressure regulating valve 15 and a solution flow control device are arranged on the pipeline.
Specifically, the solution flow control means employs a peristaltic pump 13, and the active ingredient solution is stored in a storage tank 12, and high-pressure air is supplied from an air compressor 14.
The active component solution is blown into the fluidized bed through the two-fluid nozzle 7 in the form of atomized small droplets by controlling the flow rate of the active component solution by means of the peristaltic pump 13, the pressure of the high-pressure air by means of the air compressor 14 and by means of the pressure regulating valve 15.
Specifically, the upper part of the bed body is provided with a bag-type dust collector 1, and the outlet end of the bag-type dust collector is connected with a flowmeter 16 and an induced draft fan 17. An air filter 9 and an electric heater 10 are connected to the inlet end of an air chamber 11 at the lower part of the bed body, and a thermometer 8 is arranged on a pipeline to monitor the temperature of the fluidized air. Under the action of negative pressure, the fluidized air enters an air chamber 11 through an air filter 9 and an electric heater 10 in sequence, and enters the fluidized bed conical barrel 4 through an air distribution plate to fluidize carrier particles. The draught fan 17 controls the wind speed of the fluidized wind, so that the small droplets of the active component solution are immersed into the inner pore channels on the surfaces of the porous carrier particles and are carried on the carrier after being evaporated.
Specifically, a thermocouple is inserted into a dense phase region in the fluidized bed, so that the temperature of the bed body can be detected in real time. The temperature of the bed is maintained at a suitable temperature to meet the temperature conditions required by the load.
Specifically, the top of the conical barrel 4 extends upwards to form the circular barrel 2. To facilitate observation of the fluidized state, the cylindrical drum 2 may be provided to be transparent.
The method for producing the supported carbon dioxide solid adsorbent of the present application will be further described below with reference to specific examples in conjunction with the production apparatus described above.
The first embodiment is as follows:
a preparation method of a supported carbon dioxide solid adsorbent comprises the following steps:
300g of porous alumina particles having an average particle size distribution of 0.8mm to 1mm were sieved out by a vibrating sieve, placed in a drying oven, dried at 110 ℃ for 30min and cooled to room temperature.
138g of sodium carbonate and 23g of potassium carbonate are respectively weighed by a balance, 805g of deionized water is weighed by a beaker to prepare a mixed solution, and the mass concentration of the solution is 16.7%.
The porous alumina particles are placed in a fluidized bed for continuous fluidization, and atomized air of the mixed solution of sodium carbonate and potassium carbonate is continuously introduced into the bed body through a two-fluid nozzle in the middle of an air distribution plate. Specifically, the precision peristaltic pump uniformly and stably controls the flow rate of the solution sprayed into the two-fluid nozzle to be maintained at 7.2g/min. Air with the pressure of 0.03Mpa enters the two-fluid nozzle to be mixed with the solution, so that the solution is atomized into small liquid drops to enter the bed body.
And a thermocouple is inserted into the dense-phase region of the bed body, and the temperature of the bed body is detected in real time. The air preheater controls the temperature of the fluidized air, and the temperature of the bed body is set to be about 50 ℃. The wind speed of the fluidized wind is controlled by the induced draft fan to be maintained at 1.86m/s. So that the solution droplets are impregnated into the interior of the particles on the surface of the porous alumina while the droplets are evaporating.
And (4) completely spraying the solution into the bed body, ending fluidization, and taking out the loaded alumina particles. And placing the loaded alumina particles in a muffle furnace for drying, calcining and activating, wherein the heating rate is determined to be 100 ℃/30min, and when the temperature is increased to 400 ℃, the temperature is maintained for 4 hours. And obtaining the carbon dioxide carrier adsorbent after calcining and sintering.
The solution loading time in this example was 135min.
Example two:
and keeping the rest parameters unchanged in the first embodiment, and setting the temperature of the bed body at about 20 ℃ to prepare the carbon dioxide carrier adsorbent.
Comparing the obtained adsorbent particles with the examples, when the rest parameters are unchanged, the bed temperature is reduced, the drying strength of spray liquid drops on the surface of the porous particles is reduced, and the loading depth of the active components is increased. Conversely, the active component loading depth is reduced.
Example three:
the other parameters in the first example were kept constant, and the fluidizing air speed was set at 3.87m/s to prepare a carbon dioxide carrier adsorbent.
Comparing the obtained adsorbent particles with the examples, when the other parameters are unchanged, the fluidization air speed is increased, the heat and mass transfer rate of spray liquid drops on the surfaces of the porous particles is increased, the drying strength is increased, and the loading depth of the active components is reduced. Conversely, the fluidization air velocity decreases and the active ingredient loading depth increases.
Example four:
a preparation method of a supported carbon dioxide solid adsorbent comprises the following steps:
300g of porous alumina particles having an average particle size distribution of 0.8mm to 1mm were sieved out by a vibrating sieve, placed in a drying oven, dried at 110 ℃ for 30min and cooled to room temperature.
92.6g of sodium carbonate and 15.4g of potassium carbonate are respectively weighed by a balance, 540g of deionized water is weighed by a beaker to prepare a mixed solution, and the mass concentration of the solution is 16.7%.
The porous alumina particles are placed in a fluidized bed for continuous fluidization, and atomized air of the mixed solution of sodium carbonate and potassium carbonate is continuously introduced into the bed body through a two-fluid nozzle in the middle of an air distribution plate. Specifically, the precision peristaltic pump uniformly and stably controls the flow rate of the solution sprayed into the two-fluid nozzle to be maintained at 7.2g/min. Air with the pressure of 0.03Mpa enters the two-fluid nozzle to be mixed with the solution, so that the solution is atomized into small liquid drops to enter the bed body.
And a thermocouple is inserted into the dense-phase region of the bed body, and the temperature of the bed body is detected in real time. The air preheater controls the temperature of the fluidized air, and the temperature of the bed body is set at about 50 ℃. The wind speed of the fluidized wind is controlled by the induced draft fan to be maintained at 1.86m/s. So that the solution droplets are impregnated into the interior of the particles on the surface of the porous alumina while the droplets are evaporating.
And (4) completely spraying the solution into the bed body, ending fluidization, and taking out the loaded alumina particles. And placing the loaded alumina particles in a muffle furnace for drying, calcining and activating, wherein the heating rate is determined to be 100 ℃/30min, and when the temperature is increased to 400 ℃, the temperature is maintained for 4 hours. And after calcining, obtaining the carbon dioxide carrier adsorbent.
The active ingredient solution loading time of this example was 90min.
When the obtained adsorbent particles are compared with the examples, and when the rest parameters are unchanged, the loading time is increased, the diffusion time of spray droplets in the porous particles is increased, and the loading depth of the active component is increased. Conversely, the loading time is reduced and the active ingredient loading depth is reduced.
Example five:
a preparation method of a supported carbon dioxide solid adsorbent comprises the following steps:
sieving out 300g of porous alumina particles with average particle size distribution of 0.8-1 mm by using a vibrating screen, placing the porous alumina particles in a drying oven, drying the porous alumina particles for 30min at 110 ℃, and cooling the porous alumina particles to room temperature.
92.5g of sodium carbonate and 15.5g of potassium carbonate are respectively weighed by a balance, 900g of deionized water is weighed by a beaker to prepare a mixed solution, and the mass concentration of the solution is 10%.
And placing the porous alumina particles in a fluidized bed for continuous fluidization, and introducing atomized air of a sodium carbonate and potassium carbonate mixed solution into the bed body in an intermittent liquid spraying mode through a double-fluid nozzle in the middle of an air distribution plate. Specifically, the precision peristaltic pump uniformly and stably controls the flow rate of the solution sprayed into the two-fluid nozzle to be maintained at 7.2g/min. Air with pressure of 0.03Mpa enters into the two-fluid nozzle to mix with the solution, so that the solution is atomized into small droplets and enters into the bed body, after spraying liquid for 25min each time, the peristaltic pump and the atomization air are closed for 20min, and then the liquid spraying is sequentially carried out for 25 min. The fluidized wind is maintained unchanged.
And a thermocouple is inserted into the dense-phase region of the bed body, and the temperature of the bed body is detected in real time. The air preheater controls the temperature of the fluidized air, and the temperature of the bed body is set at about 50 ℃. The wind speed of the fluidized wind is controlled by the induced draft fan to be maintained at 1.86m/s. So that the solution droplets are impregnated into the interior of the particles on the surface of the porous alumina while the droplets are evaporating.
And (4) completely spraying the solution into the bed body, ending fluidization, and taking out the loaded alumina particles. And placing the loaded alumina particles in a muffle furnace for drying, calcining and activating, wherein the heating rate is determined to be 100 ℃/30min, and when the temperature is increased to 400 ℃, the temperature is maintained for 4 hours. And obtaining the carbon dioxide carrier adsorbent after calcining and sintering.
The active ingredient solution loading time of this example was 250min.
In this example, the impregnation depth of the active component into the porous particles can also be effectively controlled by the use of a batch-type liquid spray.
According to the preparation method of the supported carbon dioxide solid adsorbent, the supported depth of the active component in the carrier can be adjusted by controlling the drying strength. The active component is prevented from being loaded at a position too deep in the pore channel, and the phenomenon that the active component cannot fully react with the carbon dioxide due to diffusion resistance in the pore channel when the carbon dioxide is adsorbed is avoided.
Compared with the traditional isometric solution impregnation method, the method has the advantages that the active component solution is atomized into small liquid drops and then is immersed into the carrier pore channel, so that the phenomenon of crystal nucleus combination in the solution evaporation process is weakened, the crystal size and the morphology are improved, the crystal quantity is more than that of the traditional preparation method, the exposed surface is effectively increased, the adsorption capacity of the adsorbent can be effectively improved, and the decarburization energy consumption is reduced.
Those of ordinary skill in the art will understand that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (6)

1. A preparation method of a supported carbon dioxide solid adsorbent is characterized by comprising the following steps:
high-temperature air is used as a fluidizing medium to lead the porous carrier particles to be circularly fluidized in the fluidized bed;
spraying the active component solution into the fluidized bed from the bottom of the bed after atomization, and immersing atomized liquid drops into porous carrier particle pore channels;
the high-temperature air is simultaneously used as a drying medium to evaporate active component liquid drops immersed into the porous carrier pore channel, the active component is loaded on the pore channel wall surface of the porous carrier particles, and the evaporation rate of the active component liquid drops in the carrier pore channel is controlled by adjusting the drying strength, so that the loading depth of the active component liquid drops in the pore channel is controlled;
calcining the loaded particles to obtain a loaded carbon dioxide solid adsorbent;
the preparation method is based on a preparation device of a load type carbon dioxide solid adsorbent, and comprises a fluidized bed body, wherein a flow guide pipe is arranged in the fluidized bed body, is coaxially arranged with the central shaft of the fluidized bed body, and is close to an air distribution plate at the bottom of the fluidized bed body; the flow guide pipe is used for guiding the fluidization direction of the porous carrier particles; the double-fluid nozzle penetrates through the air distribution plate and is aligned with the lower end opening of the flow guide pipe; the two-fluid nozzle is used for spraying atomized liquid drops of the active component; the double-fluid nozzle is simultaneously connected with high-pressure air and active component solution through a pipeline, and an air pressure regulating valve and a solution flow control device are arranged on the pipeline.
2. The method for preparing the supported carbon dioxide solid adsorbent according to claim 1, wherein the active component solution is atomized and continuously or intermittently sprayed into the fluidized bed.
3. The method for preparing a supported carbon dioxide solid adsorbent according to claim 1, wherein the porous support particles are gamma alumina; the active component solution is a mixed solution of sodium carbonate and potassium carbonate.
4. The preparation method of the supported carbon dioxide solid adsorbent according to claim 1, wherein in the preparation process, the temperature of the fluidized bed is controlled within the range of 20-70 ℃, the velocity of the fluidized medium is controlled within the range of 0.95-3.87 m/s, and the loading time of the active component solution is controlled within the range of 90-250 min.
5. The method for preparing a supported carbon dioxide solid adsorbent according to claim 1, wherein the porous carrier particles are placed in a drying oven to be completely dried and cooled before being supported.
6. The preparation method of the supported carbon dioxide solid adsorbent according to claim 1, wherein a bag-type dust remover is arranged at the top of the fluidized bed body.
CN202210190647.XA 2022-02-28 2022-02-28 Preparation method and device of supported carbon dioxide solid adsorbent Active CN114632406B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210190647.XA CN114632406B (en) 2022-02-28 2022-02-28 Preparation method and device of supported carbon dioxide solid adsorbent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210190647.XA CN114632406B (en) 2022-02-28 2022-02-28 Preparation method and device of supported carbon dioxide solid adsorbent

Publications (2)

Publication Number Publication Date
CN114632406A CN114632406A (en) 2022-06-17
CN114632406B true CN114632406B (en) 2023-03-17

Family

ID=81946886

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210190647.XA Active CN114632406B (en) 2022-02-28 2022-02-28 Preparation method and device of supported carbon dioxide solid adsorbent

Country Status (1)

Country Link
CN (1) CN114632406B (en)

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0549918A (en) * 1991-08-10 1993-03-02 Kuraray Chem Corp Carbon dioxide adsorbent
DE102007025356A1 (en) * 2007-05-31 2009-01-08 Süd-Chemie AG Process for the preparation of a coated catalyst and coated catalyst
CN102784589B (en) * 2012-09-03 2014-03-19 青岛科技大学 Nonmetal particle fluidized bed coating device and method for waste circuit board
CN103480273A (en) * 2013-09-30 2014-01-01 东南大学 Highly-activity sodium-based solid carbon dioxide absorbent
CN104588126B (en) * 2013-11-03 2017-07-28 中国石油化工股份有限公司 A kind of immersion system and the method for preparing catalyst
CN107837825A (en) * 2017-11-30 2018-03-27 西安凯立新材料股份有限公司 A kind of spraying prepares the device and method of loaded catalyst
EP3868842B1 (en) * 2020-02-19 2023-06-07 University of Limerick Particle coating method
CN111514886A (en) * 2020-04-27 2020-08-11 浙江工商大学 Medium-low temperature SCR denitration catalyst with composite microsphere structure and application thereof
CN113797856A (en) * 2021-09-23 2021-12-17 中北大学 Supergravity rotating fluidized field enhanced liquid-solid adsorption equipment and method

Also Published As

Publication number Publication date
CN114632406A (en) 2022-06-17

Similar Documents

Publication Publication Date Title
RU2659271C1 (en) Device for rapid processing of volatile organic exhaust gas and method for treating volatile organic gas
CN105772075B (en) A kind of MnOx/ SAPO-34 low-temperature SCR catalyst for denitrating flue gas and the preparation method and application thereof
CN109603459A (en) A kind of low-temperature dry fume desulfurizing agent and its preparation method and application
CN107837826B (en) Regeneration process method of inactivated flue gas denitration catalyst
CN106076417A (en) Charcoal base heteropolyacid catalyst and preparation and application method thereof for low-temperature flue gas simultaneous SO_2 and NO removal
CN109224874A (en) Catalytic membrane for air purification and preparation method thereof
CN114632406B (en) Preparation method and device of supported carbon dioxide solid adsorbent
CN108380175A (en) A kind of carbonic acid gas lanthanum-halloysite composite material and its preparation method and application
CN101791538A (en) Method for removing phenol in aqueous solution through loaded copper oxide mesoporous carbon material
WO2023061077A1 (en) High-dispersion in-situ reduction noble metal-based diesel vehicle oxidation catalyst
CN108525637A (en) A kind of carbon template modified calcium-base carbon dioxide absorber and preparation method thereof
CN104258702B (en) A kind of method of desulfurizing and denitrifying flue gas by electron beam and device
CN107961757A (en) A kind of high activity composite calcium-base CO2Absorbent and preparation method thereof
CN110394145B (en) Spherical Li4SiO4Radical CO2Method for preparing adsorbent
CN115430363B (en) Carbon dioxide capturing method and carbonator
CN108579756A (en) One main laminaria shape Mn-Fe bimetallic oxide load Cs eO2Catalyst and preparation method and application
CN114713814B (en) Preparation method of core-shell structure carbon-coated silver-zinc nanoparticle antibacterial material
CN109529808A (en) A kind of preparation method improving charcoal base SCR catalyst low temperature active
CN106178831B (en) A kind of activation of adsorbent and injection demercuration integral method
CN113247942B (en) Preparation method and application of nano copper oxide
CN115041001A (en) Electron beam ammonia flue gas desulfurization and denitrification reaction tower, device and process
JPH11347349A (en) Exhaust gas desulfurizing method and apparatus
CN106861601B (en) A kind of CO of ytterbium doping2Adsorbent and preparation method thereof
CN107867686A (en) Based on Co2C prepares the hollow nanostructured method of graphitization
CN115025751B (en) System and method for preparing adsorption material from carbon dioxide absorbent waste liquid and fly ash

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant