CN113318698A - Alkali metal loaded ceramic catalytic filler and preparation method thereof - Google Patents

Alkali metal loaded ceramic catalytic filler and preparation method thereof Download PDF

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Publication number
CN113318698A
CN113318698A CN202110730516.1A CN202110730516A CN113318698A CN 113318698 A CN113318698 A CN 113318698A CN 202110730516 A CN202110730516 A CN 202110730516A CN 113318698 A CN113318698 A CN 113318698A
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filler
alkali metal
porous ceramic
drying
ceramic filler
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蔡铭
程广文
杨嵩
赵瀚辰
杨成龙
李阳
郭中旭
付康丽
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Xian Thermal Power Research Institute Co Ltd
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Xian Thermal Power Research Institute Co Ltd
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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/30—Loose or shaped packing elements, e.g. Raschig rings or Berl saddles, for pouring into the apparatus for mass or heat transfer
    • 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
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • B01J23/04—Alkali metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/80—Organic bases or salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/202—Alkali metals
    • B01D2255/2022—Potassium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/204—Alkaline earth metals
    • B01D2255/2047—Magnesium
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • 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
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Abstract

The invention discloses an alkali metal loaded ceramic catalytic filler and a preparation method thereof, the alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, the active component comprises alkali metal ions and magnesium oxide, the filler can accelerate the rate of tertiary amine absorbing carbon dioxide, and can avoid the problems of insufficient space of an absorption tower, overweight internal parts and gas-liquid flow, and the preparation method is simple.

Description

Alkali metal loaded ceramic catalytic filler and preparation method thereof
Technical Field
The invention belongs to the technical field of emission reduction of greenhouse gas carbon dioxide, and relates to an alkali metal loaded ceramic catalytic filler and a preparation method thereof.
Background
The chemical absorption method is more commonly used, organic amine mainly comprises primary amine (such as MEA), secondary amine (such as DEA) and tertiary amine (such as MDEA, TEA and the like), the primary amine and the secondary amine react with carbon dioxide relatively quickly, and the generated carbamate has relatively stable chemical property, but has the defects of small saturated capacity of the carbon dioxide, large heat of desorption reaction and the like; compared with primary amine and secondary amine, the tertiary amine has large carbon dioxide saturation capacity and small heat of desorption reaction, but because the N atom of the tertiary amine does not contain active hydrogen, the tertiary amine can only indirectly react with CO2The rate of absorption of carbon dioxide by tertiary amines is relatively slow as a result of molecular reactions.
The organic amine solution chemical absorption of carbon dioxide usually adopts a filler absorption tower, and stainless steel, plastic or ceramic filler is arranged in the absorption tower to increase the gas-liquid contact area and the mass transfer efficiency. If the catalyst and the filler are respectively arranged in the absorption tower, the problems of insufficient space, heavy internal parts, gas-liquid flow and the like of the absorption tower can be caused.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an alkali metal-loaded ceramic catalytic filler and a preparation method thereof, wherein the filler can accelerate the rate of tertiary amine absorbing carbon dioxide, can avoid the problems of insufficient space of an absorption tower, overweight internal parts and gas-liquid flow, and is simple in preparation method.
In order to achieve the above object, the alkali metal-loaded ceramic catalytic filler of the present invention comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler or foam porous ceramic filler.
The porous ceramic filler is pall ring, Raschig ring, ceramic ball or corrugated plate.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) pretreating the porous ceramic filler;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 5-20%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 5-20%;
3) immersing the porous ceramic filler in Mg salt solution, and then carrying out ultrasonic impregnation, drying, calcining and cooling;
4) immersing the porous ceramic filler treated in the step 3) in an alkali solution, and then carrying out ultrasonic impregnation, drying, calcining and cooling to obtain the alkali metal loaded ceramic catalytic filler.
The magnesium salt is magnesium nitrate hexahydrate or magnesium acetate tetrahydrate.
The alkali metal hydroxide is NaOH or KOH.
The specific operation process of the step 1) is as follows:
removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing liquid is 7, and finally drying for 12h in an oven at the temperature of 110 ℃.
The specific operation process of the step 3) is as follows:
immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 2-4 times, wherein the ultrasonic impregnation is carried out for 1-3 h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500-fold at the heating rate of 5 ℃/min under the atmosphere of inert gas, calcining at constant temperature for 2h, and then naturally cooling to room temperature under the atmosphere of inert gas.
The specific operation of the step 4) is as follows:
immersing the calcined porous ceramic filler in an alkali solution, performing ultrasonic impregnation and drying for 2-4 times, wherein the ultrasonic impregnation is performed for 1-3 h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500-fold at the heating rate of 5 ℃/min under the atmosphere of inert gas, calcining at constant temperature for 2h, and then naturally cooling to room temperature under the atmosphere of inert gas to obtain the alkali metal loaded ceramic catalytic filler.
The invention has the following beneficial effects:
the alkali metal loaded ceramic catalytic filler and the preparation method thereof have the advantages that during specific operation, the active component is attached to the porous ceramic filler, and the CO is accelerated while the gas-liquid distribution and mass transfer functions of the conventional filler are not influenced2The reaction rate with organic amine molecules is increased, and CO is increased2The absorption speed and the absorption capacity of the organic amine, and the solution of organic amine absorption solvent and CO2Low reaction speed, high energy consumption and the like, and can reduce CO2The amine solvent circulation amount of the trapping device, the system power consumption and the subsequent solution heating regeneration steam consumption. Meanwhile, a catalyst and a filler do not need to be separately arranged in the absorption tower, so that the problems of insufficient space of the absorption tower, overweight internal parts and gas-liquid flow are avoided, and in addition, the preparation method is simpler by adopting the processes of ultrasonic impregnation, drying and calcination.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following will clearly and completely describe the technical solution of the present invention with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments, and are not intended to limit the scope of the disclosure of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present disclosure. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler or foam porous ceramic filler.
The porous ceramic filler is pall ring, Raschig ring, ceramic ball or corrugated plate.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) pretreating the porous ceramic filler;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 5-20%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 5-20%;
3) immersing the porous ceramic filler in Mg salt solution, and then carrying out ultrasonic impregnation, drying, calcining and cooling;
4) immersing the porous ceramic filler treated in the step 3) in an alkali solution, and then carrying out ultrasonic impregnation, drying, calcining and cooling to obtain the alkali metal loaded ceramic catalytic filler.
The magnesium salt is magnesium nitrate hexahydrate or magnesium acetate tetrahydrate.
The alkali metal hydroxide is NaOH or KOH.
The specific operation process of the step 1) is as follows:
removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing liquid is 7, and finally drying for 12h in an oven at the temperature of 110 ℃.
The specific operation process of the step 3) is as follows:
immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 2-4 times, wherein the ultrasonic impregnation is carried out for 1-3 h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500-fold at the heating rate of 5 ℃/min under the atmosphere of inert gas, calcining at constant temperature for 2h, and then naturally cooling to room temperature under the atmosphere of inert gas.
The specific operation of the step 4) is as follows:
immersing the calcined porous ceramic filler in an alkali solution, performing ultrasonic impregnation and drying for 2-4 times, wherein the ultrasonic impregnation is performed for 1-3 h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500-fold at the heating rate of 5 ℃/min under the atmosphere of inert gas, calcining at constant temperature for 2h, and then naturally cooling to room temperature under the atmosphere of inert gas to obtain the alkali metal loaded ceramic catalytic filler.
Example one
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler.
The porous ceramic filler is pall ring.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 10%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 20%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 3 times, wherein the ultrasonic impregnation is carried out for 2 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then heating to 600 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2 hours, and then naturally cooling to the room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 3 times, wherein the ultrasonic immersing is carried out for 1h-3h, the drying temperature is 110 ℃, the drying time is 12h, then the temperature is raised to 600 ℃ at the temperature raising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is carried out for 2h, and then the natural cooling is carried out to the room temperature under the atmosphere of inert gas, so as to obtain the alkali metal loaded ceramic catalytic filler, and obtain the alkali metal loaded ceramic catalytic filler.
The magnesium salt is magnesium nitrate hexahydrate.
The alkali metal hydroxide is KOH.
Example two
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is foam porous ceramic filler.
The porous ceramic filler is pall ring.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 15%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 10%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 2 times, wherein the ultrasonic impregnation is carried out for 2 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then heating to 600 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2 hours, and then naturally cooling to the room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 2 times, wherein the ultrasonic immersing is carried out for 2 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then the temperature is raised to 600 ℃ at the temperature raising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is carried out for 2 hours, and then the natural cooling is carried out to the room temperature under the atmosphere of inert gas, so as to obtain the ceramic catalytic filler loaded by alkali metal, and obtain the ceramic catalytic filler loaded by alkali metal.
The magnesium salt is magnesium nitrate hexahydrate.
The alkali metal hydroxide is KOH.
EXAMPLE III
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler.
The porous ceramic filler is Raschig ring.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 10%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 10%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 3 times, wherein the ultrasonic impregnation is carried out for 2 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then heating to 600 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2 hours, and then naturally cooling to the room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 2 times, wherein the ultrasonic immersing is carried out for 2 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then the temperature is raised to 600 ℃ at the temperature raising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is carried out for 2 hours, and then the natural cooling is carried out to the room temperature under the atmosphere of inert gas, so as to obtain the ceramic catalytic filler loaded by alkali metal, and obtain the ceramic catalytic filler loaded by alkali metal.
The magnesium salt is magnesium acetate tetrahydrate.
The alkali metal hydroxide is KOH.
Example four
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is foam porous ceramic filler.
The porous ceramic filler is Raschig ring.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 15%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 20%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 3 times, wherein the ultrasonic impregnation is carried out for 2 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then heating to 600 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2 hours, and then naturally cooling to the room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 3 times, wherein the ultrasonic immersing is carried out for 2 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then the temperature is raised to 600 ℃ at the temperature raising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is carried out for 2 hours, and then the natural cooling is carried out to the room temperature under the atmosphere of inert gas, so as to obtain the ceramic catalytic filler loaded by alkali metal, and obtain the ceramic catalytic filler loaded by alkali metal.
The magnesium salt is magnesium acetate tetrahydrate.
The alkali metal hydroxide is KOH.
Comparative example 1
This comparative example provides a catalyst-free ceramic blank comprising the steps of:
1) selecting phi 25 pall ring porous ceramic filler, removing surface impurities, pretreating the porous ceramic filler by adopting an oxalic acid solution with the mass fraction of 30%, and carrying out condensation reflux boiling for 1 h; cooling, washing with deionized water until the pH value of the washing liquid is 7, and drying in an oven at 110 ℃ for 12h for later use;
2) and (3) heating the dried ceramic filler to 600 ℃ in a muffle furnace at a heating rate of 5 ℃/min under the atmosphere of inert gas, calcining for 2h, and naturally cooling to room temperature under the atmosphere of inert gas to obtain the hollow ceramic filler.
Comparative example No. two
The comparative example provides a method for preparing an alkali metal-loaded ceramic catalytic filler, comprising the steps of:
1) selecting phi 25 pall ring porous ceramic filler, removing surface impurities, pretreating the porous ceramic filler by adopting an oxalic acid solution with the mass fraction of 30%, and carrying out condensation reflux boiling for 1 h; cooling, washing with deionized water until the pH value of the washing liquid is 7, and drying in an oven at 110 ℃ for 12h for later use;
2) 209g of magnesium nitrate hexahydrate (Mg (NO) were taken3)2.6H2O) is put into a container, 1L of deionized water is added, the mixture is stirred until the deionized water is completely dissolved, and Mg (NO) with the mass concentration of 10 percent is prepared3)2Solution, denoted as solution a 6.
3) Immersing the ceramic filler in the solution A6, ultrasonically immersing for 2h, and then placing the immersed ceramic filler in an oven to dry for 12h at 110 ℃; repeating the soaking and drying for 3 times; heating the soaked and dried ceramic filler to 600 ℃ at a heating rate of 5 ℃/min in an inert gas atmosphere in a muffle furnace, calcining for 2h, and naturally cooling to room temperature in the inert gas atmosphere to obtain the MgO-loaded ceramic filler;
small CO in laboratory for ceramic fillers prepared in examples one to two2Absorption evaluation device for effect verification, CO2The absorption tower used by the absorption evaluation device is a stainless steel reactor with the inner diameter of 95mm, random packing is filled, the length of the packing section is 1m, and a heat insulation layer is arranged outside the absorption tower. The measurement conditions adopted by the present invention are as follows: carbon dioxide (CO)2) 12% by volume of nitrogen (N)2) The volume fraction is 88 percent, and the gas amount is 8L/min; the liquid-gas ratio is 5L/m3(ii) a The temperature of the absorption liquid is 50 ℃; for comparison, the absorption liquid used for evaluation is a newly prepared organic amine aqueous solution and consists of MEA with 5% of mass concentration and MDEA with 15% of mass concentration.
When the reaction conditions are stably achieved, continuously measuring the CO in the outlet gas of the packed tower2Volume fraction and rich liquid CO at rich liquid outlet at bottom of packed tower2Load, CO2The absorption efficiency calculation formula is:
the removal efficiency is high (original flue gas CO)2Volume concentration of raw flue gas flow-clean flue gas CO2Volume concentration net flue gas flow)/(raw flue gas CO2Volume concentration x primary flue gas flow) x 100%;
absorption liquid CO2Absorption liquid CO2Molarity/molarity of solution absorbent;
absorption liquid CO2The molar concentration is obtained by chemical analysis of the excess acid reaction, and the molar concentration of the absorbent is obtained by acid-base titration.
In the effect verification experiment, the pall ring or raschig ring packing loaded in the absorption tower is the CP1, CP2, CP3 and CP4 loaded ceramic packing prepared in the first to fourth examples, and the packing loaded in the first and second comparative absorption towers is the CP5 and CP6 comparative ceramic packing respectively, the volume and other conditions of the packing are the same, and the effect verification result is shown in table 1.
TABLE 1
Figure BDA0003139173110000121
Figure BDA0003139173110000131
As can be seen from Table 1, the first to fourth examples enhance the CO content of the MDEA/MEA solution by using the K/MgO-loaded ceramic filler, as compared to the blank ceramic filler of the first comparative example, which is not loaded, and the MgO-only ceramic filler of the second comparative example2Absorption performance, absorption efficiency in absorption column and CO of solution2The load is obviously improved.
EXAMPLE five
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is foam porous ceramic filler.
The porous ceramic filler is ceramic balls.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 5%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 5%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 2 times, wherein the ultrasonic impregnation is carried out for 1h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2h, and then naturally cooling to room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 2 times, wherein the ultrasonic immersing is performed for 1h, the drying temperature is 110 ℃, the drying time is 12h, then the temperature is increased to 500 ℃ at the temperature rising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is performed for 2h, and then the natural cooling is performed to the room temperature under the atmosphere of inert gas, so that the alkali metal loaded ceramic catalytic filler is obtained, and the alkali metal loaded ceramic catalytic filler is obtained.
The magnesium salt is magnesium acetate tetrahydrate.
The alkali metal hydroxide is NaOH.
EXAMPLE six
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler.
The porous ceramic filler is a corrugated plate.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 20%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 20%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 4 times, wherein the ultrasonic impregnation is carried out for 3 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then heating to 700 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2 hours, and then naturally cooling to the room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 4 times, wherein the ultrasonic immersing is carried out for 3 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then the temperature is raised to 700 ℃ at the temperature raising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is carried out for 2 hours, and then the natural cooling is carried out to the room temperature under the atmosphere of inert gas, so as to obtain the ceramic catalytic filler loaded by alkali metal, and obtain the ceramic catalytic filler loaded by alkali metal.
The magnesium salt is magnesium acetate tetrahydrate.
The alkali metal hydroxide is KOH.
EXAMPLE seven
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler.
The porous ceramic filler is a corrugated plate.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 15%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 15%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 3 times, wherein the ultrasonic impregnation is carried out for 2.5 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then heating to 650 ℃ at the heating rate of 5 ℃/min under the atmosphere of inert gas, then carrying out constant-temperature calcination for 2 hours, and then naturally cooling to room temperature under the atmosphere of inert gas;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 3 times, wherein the ultrasonic immersing is carried out for 2.5 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then the temperature is raised to 650 ℃ at the temperature raising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is carried out for 2 hours, and then the natural cooling is carried out to the room temperature under the atmosphere of inert gas, so as to obtain the ceramic catalytic filler loaded by alkali metal, and obtain the ceramic catalytic filler loaded by alkali metal.
The magnesium salt is magnesium acetate tetrahydrate.
The alkali metal hydroxide is NaOH.
Example eight
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler.
The porous ceramic filler is ceramic balls.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare an Mg salt solution with the mass percentage concentration of 8%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 8%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 4 times, wherein the ultrasonic impregnation is carried out for 1.5h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 550 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2h, and then naturally cooling to the room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 4 times, wherein the ultrasonic immersing is performed for 1.5h, the drying temperature is 110 ℃, the drying time is 12h, then the temperature is increased to 550 ℃ at the temperature rising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is performed for 2h, and then the natural cooling is performed to the room temperature under the atmosphere of inert gas, so that the alkali metal loaded ceramic catalytic filler is obtained, and the alkali metal loaded ceramic catalytic filler is obtained.
The magnesium salt is magnesium acetate tetrahydrate.
The alkali metal hydroxide is NaOH.
Example nine
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is foam porous ceramic filler.
The porous ceramic filler is Raschig ring.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 10%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 10%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 2 times, wherein the ultrasonic impregnation is carried out for 3 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then heating to 700 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2 hours, and then naturally cooling to the room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 2 times, wherein the ultrasonic immersing is carried out for 3 hours, the drying temperature is 110 ℃, the drying time is 12 hours, then the temperature is raised to 700 ℃ at the temperature raising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is carried out for 2 hours, and then the natural cooling is carried out to the room temperature under the atmosphere of inert gas, so as to obtain the ceramic catalytic filler loaded by alkali metal, and obtain the ceramic catalytic filler loaded by alkali metal.
The magnesium salt is magnesium nitrate hexahydrate.
The alkali metal hydroxide is NaOH.
Example ten
The alkali metal loaded ceramic catalytic filler comprises a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
The porous ceramic filler is honeycomb porous ceramic filler.
The porous ceramic filler is pall ring.
The alkali metal-loaded ceramic catalytic filler is applied to an absorption tower for chemically absorbing carbon dioxide by organic amine.
The preparation method of the alkali metal loaded ceramic catalytic filler comprises the following steps:
1) removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing solution is 7, and finally drying for 12h in an oven at the temperature of 110 ℃;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 5%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 20%;
3) immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 4 times, wherein the ultrasonic impregnation is carried out for 1h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500 ℃ at the heating rate of 5 ℃/min under the inert gas atmosphere, then carrying out constant-temperature calcination for 2h, and then naturally cooling to room temperature under the inert gas atmosphere;
4) immersing the calcined porous ceramic filler in an alkali solution, and then ultrasonically immersing and drying for 4 times, wherein the ultrasonic immersing is performed for 1h, the drying temperature is 110 ℃, the drying time is 12h, then the temperature is increased to 500 ℃ at the temperature rising speed of 5 ℃/min under the atmosphere of inert gas, then the constant-temperature calcining is performed for 2h, and then the natural cooling is performed to the room temperature under the atmosphere of inert gas, so that the alkali metal loaded ceramic catalytic filler is obtained, and the alkali metal loaded ceramic catalytic filler is obtained.
The magnesium salt is magnesium acetate tetrahydrate.
The alkali metal hydroxide is KOH.

Claims (10)

1. An alkali metal supported ceramic catalytic filler comprising a porous ceramic filler and an active component attached to the porous ceramic filler, wherein the active component comprises alkali metal ions and magnesium oxide.
2. The alkali metal supported ceramic catalytic filler of claim 1, wherein the porous ceramic filler is a honeycomb porous ceramic filler or a foam porous ceramic filler.
3. The alkali metal-loaded ceramic catalytic filler according to claim 1, wherein the porous ceramic filler is a pall ring, a raschig ring, a ceramic ball or a corrugated plate.
4. The method of making an alkali metal-loaded ceramic catalytic filler according to claim 1, wherein the alkali metal-loaded ceramic catalytic filler is applied in an absorption column for the chemical absorption of carbon dioxide by organic amines.
5. A method of making an alkali metal supported ceramic catalytic filler as claimed in claim 1, comprising the steps of:
1) pretreating the porous ceramic filler;
2) adding Mg salt into deionized water to prepare a Mg salt solution with the mass percentage concentration of 5-20%; adding alkali metal hydroxide into deionized water to prepare an alkali solution with the mass percentage concentration of 5-20%;
3) immersing the porous ceramic filler in Mg salt solution, and then carrying out ultrasonic impregnation, drying, calcining and cooling;
4) immersing the porous ceramic filler treated in the step 3) in an alkali solution, and then carrying out ultrasonic impregnation, drying, calcining and cooling to obtain the alkali metal loaded ceramic catalytic filler.
6. The method of making an alkali metal supported ceramic catalytic filler as claimed in claim 5 wherein the magnesium salt is magnesium nitrate hexahydrate or magnesium acetate tetrahydrate.
7. The method of making an alkali metal supported ceramic catalytic filler according to claim 5, wherein the alkali metal hydroxide is NaOH or KOH.
8. The process for the preparation of an alkali metal supported ceramic catalytic filler according to claim 5, characterized in that the specific operating procedure of step 1) is:
removing impurities on the surface of the porous ceramic filler, cleaning the porous ceramic filler by adopting an oxalic acid solution with the mass percentage concentration of 30%, then condensing, refluxing and boiling for 1h, cooling, washing by using deionized water until the pH value of a washing liquid is 7, and finally drying for 12h in an oven at the temperature of 110 ℃.
9. The process for the preparation of an alkali metal supported ceramic catalytic filler according to claim 5, characterized in that the specific operating procedure of step 3) is:
immersing the porous ceramic filler in Mg salt solution, carrying out ultrasonic impregnation and drying for 2-4 times, wherein the ultrasonic impregnation is carried out for 1-3 h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500-fold at the heating rate of 5 ℃/min under the atmosphere of inert gas, calcining at constant temperature for 2h, and then naturally cooling to room temperature under the atmosphere of inert gas.
10. The process for the preparation of an alkali metal supported ceramic catalytic filler according to claim 5, characterized in that the specific operations of step 4) are:
immersing the calcined porous ceramic filler in an alkali solution, performing ultrasonic impregnation and drying for 2-4 times, wherein the ultrasonic impregnation is performed for 1-3 h, the drying temperature is 110 ℃, the drying time is 12h, then heating to 500-fold at the heating rate of 5 ℃/min under the atmosphere of inert gas, calcining at constant temperature for 2h, and then naturally cooling to room temperature under the atmosphere of inert gas to obtain the alkali metal loaded ceramic catalytic filler.
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