CN116272836A - Adsorbent and preparation method and application thereof - Google Patents
Adsorbent and preparation method and application thereof Download PDFInfo
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- CN116272836A CN116272836A CN202310085929.8A CN202310085929A CN116272836A CN 116272836 A CN116272836 A CN 116272836A CN 202310085929 A CN202310085929 A CN 202310085929A CN 116272836 A CN116272836 A CN 116272836A
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 53
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 43
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 43
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 32
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000292 calcium oxide Substances 0.000 claims abstract description 26
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000013067 intermediate product Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 23
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 5
- 238000001179 sorption measurement Methods 0.000 abstract description 21
- 239000002893 slag Substances 0.000 abstract description 20
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 10
- 239000003960 organic solvent Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 9
- 230000008929 regeneration Effects 0.000 abstract description 9
- 238000011069 regeneration method Methods 0.000 abstract description 9
- 238000003912 environmental pollution Methods 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 5
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- JCCZVLHHCNQSNM-UHFFFAOYSA-N [Na][Si] Chemical compound [Na][Si] JCCZVLHHCNQSNM-UHFFFAOYSA-N 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000002336 sorption--desorption measurement Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 52
- 239000001569 carbon dioxide Substances 0.000 description 26
- 229910002092 carbon dioxide Inorganic materials 0.000 description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 20
- 239000003513 alkali Substances 0.000 description 20
- 235000019738 Limestone Nutrition 0.000 description 17
- 239000006028 limestone Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 14
- 239000011575 calcium Substances 0.000 description 11
- 239000000377 silicon dioxide Substances 0.000 description 10
- 229910052791 calcium Inorganic materials 0.000 description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- 239000011734 sodium Substances 0.000 description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000002910 solid waste Substances 0.000 description 5
- 238000003915 air pollution Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000012621 metal-organic framework Substances 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical class [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910002090 carbon oxide Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 3
- 229910052815 sulfur oxide Inorganic materials 0.000 description 3
- 241000282412 Homo Species 0.000 description 2
- 239000013206 MIL-53 Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 hydroxide ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
-
- 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
- B01D53/04—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 stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application relates to an adsorbent, a preparation method and application thereof, belonging to the technical field of environmental protection; the method comprises the following steps: obtaining particles containing calcium oxide and kaolin; mixing the calcium oxide component-containing particles, kaolin particles and hydroxyl ion component-containing substances, and performing hydrothermal reaction to obtain an intermediate product; cooling the intermediate product, and then sintering to obtain an adsorbent; the method has the advantages that the method adopts the raw materials with low price in nature and high calcium carbonate content or the sodium silicon slag, the calcium silicon slag and the kaolin which can provide calcium oxide as the raw materials to synthesize the high-efficiency adsorbent with large specific surface area in situ, and compared with the mesoporous alumina adsorbent, the adsorbent can avoid adding the organic solvent, thereby avoiding the corrosion of the organic solvent participating in the reaction to equipment and the aggravation of environmental pollution under the high temperature condition, and simultaneously avoiding the factors of low recycling efficiency and the like caused by the large energy consumption, complex operation and difficult adsorption and regeneration of the whole gas in the adsorption/desorption process.
Description
Technical Field
The application relates to the technical field of environmental protection, in particular to an adsorbent and a preparation method and application thereof.
Background
One significant problem facing humans is environmental pollution. Air pollution is a major component of environmental pollution, and the emission of toxic gases such as sulfur oxides, nitrogen oxides, carbon oxides, and hydrogen sulfide gases, which are often combined with water and oxygen molecules to form acid rain, is a major factor of air pollution. Other gases, such as carbon dioxide, fluorocarbon, are more likely to escape to the outer space and destroy the ozone layer, resulting in global warming. At present, the global carbon dioxide emission has reached a critical point, the annual increasing emission is 130 hundred million tons, the current concentration of carbon dioxide in the atmosphere has reached 391.8ppm, and the sea level and human ecosystem have been affected by the large amount of carbon dioxide emissions. Although the carbon dioxide emission generated by partial self can be offset through the ways of tree planting, energy saving, emission reduction and the like, the carbon dioxide emission can be greatly reduced by adopting a carbon dioxide trapping and absorbing technology in the process of economic development, and the recycling of carbon dioxide gas is realized.
The commonly used absorbing materials at present comprise active mesoporous alumina materials and metal-organic framework materials; the active mesoporous alumina material has the advantages of porosity and high dispersibility, larger specific surface area and adsorption performance, and alpha type is a stable phase of alumina and is also a main composition of corundum, the structure is stable, the density is high, the strength is high, the active mesoporous alumina material needs to be matched with an organic solvent for use, the adsorption agent and the adsorbate desorption operation are complex in the chemical adsorption of gas, and the organic solvent which usually participates in the reaction has the corrosion of equipment and the pollution degree of the environment under the high-temperature condition, so that the energy consumption of the whole gas is high in the adsorption/desorption process, the operation is complex, the adsorbent regeneration is difficult, the recycling efficiency is low, the pollution is serious and the like. The metal-organic framework material has a special hole structure and a huge specific surface area, which is very beneficial to gas adsorption, wherein the gas adsorption performance of the MIL-53 (Al) framework material taking trivalent aluminum as a central metal ion is more and more concerned, but the hole structure and the specific surface area of the material are greatly influenced by preparation condition factors, and improvement and optimization of synthesis conditions are urgently needed to improve the thermal stability and the hole structure property of the framework structure, and further improve the adsorption capacity to gas.
Disclosure of Invention
The application provides an adsorbent, a preparation method and application thereof, and aims to solve the problems of corrosion to equipment and aggravation of environmental pollution at high temperature caused by the fact that the conventional adsorbent is matched with an organic solvent.
In a first aspect, the present application provides a method of preparing an adsorbent, the method comprising:
obtaining particles containing calcium oxide and kaolin;
mixing the calcium oxide component-containing particles, kaolin particles and hydroxyl ion component-containing substances, and performing hydrothermal reaction to obtain an intermediate product;
and cooling the intermediate product, and sintering to obtain the adsorbent.
As an alternative embodiment, the particles of the calcium oxide-containing ingredient have a molded average particle diameter of 2 to 4mm; and/or
The average particle diameter of the kaolin particles is 0.4-0.7mm.
As an alternative embodiment, the mass of the calcium oxide-containing component particles mixed per 100 milliliters of the hydroxide ion-containing component material is from 1 to 2.5 grams; and/or
The mass of the kaolin particles mixed per 100 ml of the hydroxide ion containing component material is 30-45g.
As an alternative embodiment, the mixing time of the calcium oxide-containing component particles and the hydroxide ion-containing component material is from 0.5 to 1 hour; and/or
The mixing time of the kaolin particles and the hydroxide ion component containing substance is 1.5h to 2.5h.
As an alternative embodiment, the temperature of the hydrothermal reaction is 30-300 ℃; or (b)
The temperature of the hydrothermal reaction is 50-200 ℃.
As an alternative embodiment, natural cooling is adopted for the cooling; and/or
The cooling time is 1.5-2.5h.
As an alternative embodiment, the sintering temperature is 400-900 ℃; and/or
The sintering time is 1-4h.
As an alternative embodiment, the sintering temperature is 450-550 ℃; and/or
The sintering time is 1.5-2.5h.
In a second aspect, the present application provides an adsorbent prepared by the method of preparing an adsorbent according to the first aspect.
In a third aspect, the present application provides the use of an adsorbent for the absorption of a gas, the adsorbent being in accordance with the second aspect.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the method provided by the embodiment of the application, the high-efficiency adsorbent with large specific surface area is synthesized in situ by adopting the natural cheap substances containing the calcium oxide component, the solid waste sodium silica slag containing the calcium oxide component, the calcium silica slag and the like and kaolin as raw materials, and compared with the mesoporous alumina adsorbent, the adsorbent can avoid adding an organic solvent, so that the corrosion of the organic solvent participating in the reaction on equipment and the aggravation of environmental pollution under the high-temperature condition are avoided, and meanwhile, the factors of low recycling efficiency and the like caused by the large energy consumption, complex operation and difficult adsorption and regeneration of the whole gas in the adsorption/desorption process are avoided.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a flowchart of a method provided in an embodiment of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
Unless specifically indicated otherwise, the various raw materials, reagents, instruments, equipment, and the like used in this application are commercially available or may be prepared by existing methods.
One significant problem facing humans is environmental pollution. Air pollution is a major component of environmental pollution, and the emission of toxic gases such as sulfur oxides, nitrogen oxides, carbon oxides, and hydrogen sulfide gases, which are often combined with water and oxygen molecules to form acid rain, is a major factor of air pollution. Other gases, such as carbon dioxide, fluorocarbon, are more likely to escape to the outer space and destroy the ozone layer, resulting in global warming. At present, the global carbon dioxide emission has reached a critical point, the annual increasing emission is 130 hundred million tons, the current concentration of carbon dioxide in the atmosphere has reached 391.8ppm, and the sea level and human ecosystem have been affected by the large amount of carbon dioxide emissions. Although the carbon dioxide emission generated by partial self can be offset through the ways of tree planting, energy saving, emission reduction and the like, the carbon dioxide emission can be greatly reduced by adopting a carbon dioxide trapping and absorbing technology in the process of economic development, and the recycling of carbon dioxide gas is realized.
The commonly used absorbing materials at present comprise active mesoporous alumina materials and metal-organic framework materials; the active mesoporous alumina material has the advantages of porosity and high dispersibility, larger specific surface area and adsorption performance, and alpha type is a stable phase of alumina and is also a main composition of corundum, the structure is stable, the density is high, the strength is high, the active mesoporous alumina material needs to be matched with an organic solvent for use, the adsorption agent and the adsorbate desorption operation are complex in the chemical adsorption of gas, and the organic solvent which usually participates in the reaction has the corrosion of equipment and the pollution degree of the environment under the high-temperature condition, so that the energy consumption of the whole gas is high in the adsorption/desorption process, the operation is complex, the adsorbent regeneration is difficult, the recycling efficiency is low, the pollution is serious and the like. The metal-organic framework material has a special hole structure and a huge specific surface area, which is very beneficial to gas adsorption, wherein the gas adsorption performance of the MIL-53 (Al) framework material taking trivalent aluminum as a central metal ion is more and more concerned, but the hole structure and the specific surface area of the material are greatly influenced by preparation condition factors, and improvement and optimization of synthesis conditions are urgently needed to improve the thermal stability and the hole structure property of the framework structure, and further improve the adsorption capacity to gas.
As shown in fig. 1, an embodiment of the present application provides a method for preparing an adsorbent, including:
s1, obtaining particles containing calcium oxide components and kaolin particles; the particles containing the calcium oxide component may be selected from solid waste materials such as sodium silica slag and calcium silica slag, and raw materials having a high calcium carbonate content such as calcium carbonate, dolomite, chalk, and shells.
In some embodiments, the particles of the calcium oxide-containing ingredient have an average particle size of 2-4mm; the average particle diameter of the kaolin particles is 0.4-0.7mm.
The particle size can influence the reaction speed, the particle diameters of the particles containing the calcium oxide component and the kaolin particles are controlled to be 2-4mm and 0.4-0.7mm respectively, the particle size is overlarge, the reaction speed can be reduced, and the gap size among the particles in the use process can also reduce the use efficiency and influence the purity of the substances. Too small particles can increase energy consumption.
Specifically, in this example, limestone and kaolin are crushed and sieved, the size of the limestone is 2-4mm, and the particle size of the kaolin is 0.4-0.7mm.
S2, mixing the calcium oxide component-containing particles, the kaolin particles and the hydroxyl ion component-containing substances, and performing hydrothermal reaction to obtain an intermediate product; the hydroxide ion-containing component substance may be selected from solid waste matter adhering bases such as sodium silica slag and calcium silica slag, and hydroxide ion-containing substances such as sodium hydroxide, calcium hydroxide and potassium hydroxide.
In some embodiments, the mass of the calcium oxide-containing component particles mixed per 100 milliliters of the hydroxide ion-containing component material is from 1 to 2.5 grams; the mass of the kaolin particles mixed per 100 ml of the hydroxide ion containing component material is 30-45g.
The applicant found through experiments that: the concentration of the calcium oxide-containing component particles and the hydroxide ion-containing component substances is controlled to be 1-2.5 g/100 ml;
the concentration of the kaolin particles and the hydroxide ion containing material is preferably controlled within a range of 30-45 g/100 ml.
In some embodiments, the mixing time of the calcium oxide-containing ingredient particles and the hydroxide ion-containing ingredient material is from 0.5 to 1 hour; the mixing time of the kaolin particles and the hydroxide ion component containing substance is 1.5h to 2.5h.
The applicant found through experiments that: the mixing time of the calcium oxide-containing component particles and the kaolin particles with the hydroxide ion-containing component substance is controlled to be in the preferable range of 0.5 to 1h and 1.5 to 2.5h, respectively.
In some embodiments, the temperature of the hydrothermal reaction is 30-300 ℃; preferably, the temperature of the hydrothermal reaction is 50-200 ℃.
Specifically, in this example, calcium oxide-containing component particles and kaolin particles were mixed with hydroxide ion-containing component substances of different concentrations. The hydroxide ion-containing component material may be selected from sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium silica slag, calcium silica slag, and other solid wastes capable of providing hydroxide ions. The manner of controlling the hydroxide mixed with the substance containing the calcium oxide component is as follows: the molar ratio of calcium to hydroxyl is 7-15, and the control mode of the hydroxide mixed with the kaolin particles is as follows: the molar ratio of aluminum to hydroxyl is 10-25.
S3, cooling the intermediate product, and then sintering to obtain the adsorbent.
In some embodiments, the cooling employs natural cooling; the cooling time is 1.5-2.5h.
In some embodiments, the sintering temperature is 400-900 ℃; the sintering time is 1-4h. Preferably, the sintering temperature is 450-550 ℃; the sintering time is 1.5-2.5h. More preferably, the sintering temperature is 500 ℃; the sintering time is 2h.
The sintering temperature is controlled to be 400-900 ℃ and the sintering time is controlled to be 1-4 hours, and other miscellaneous phase substances can be generated when the temperature is too high or the sintering time is too long.
The method adopts solid waste substances such as sodium silica slag, calcium silica slag and the like, natural cheap raw materials such as calcium carbonate, dolomite, chalk, shells and the like with high content of calcium carbonate and kaolin as raw materials to synthesize the high-efficiency adsorbent with large specific surface area in situ.
Based on one general inventive concept, embodiments of the present application also provide an adsorbent prepared using the method of preparing an adsorbent as provided above.
The adsorbent is prepared based on the above method, and specific steps of the method can refer to the above embodiment, and because the adsorbent adopts some or all of the technical solutions of the above embodiment, the adsorbent has at least all of the beneficial effects brought by the technical solutions of the above embodiment, and will not be described in detail herein.
Based on one general inventive concept, embodiments of the present application also provide for the use of an adsorbent for the absorption of a gas, the adsorbent being an adsorbent as provided above.
Specifically, the adsorbent is used for the absorption of acid gases, which may be specifically selected from sulfur oxides, nitrogen oxides, carbon oxides, hydrogen sulfide gases, and the like.
The adsorbent can realize the efficient trapping and absorbing technology of acid gases such as carbon dioxide, can greatly reduce the emission of carbon dioxide, and can realize the recycling of carbon dioxide.
The present application is further illustrated below in conjunction with specific examples. It should be understood that these examples are illustrative only of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
A method of preparing an adsorbent, the method comprising:
crushing limestone and kaolin, classifying according to the granularity of 4-0.5 mm, selecting 3mm limestone, controlling the concentration of limestone and alkali at 3 g/100 ml, and controlling the mixing time of limestone and alkali at 55 minutes; selecting 0.5mm kaolin, controlling the concentration of the kaolin and alkali at 38 g/100 ml, and controlling the mixing time of the kaolin and alkali at 1 hour; the mixture of limestone, kaolin and alkali is reacted in a thermal reactor for 15 minutes at 50 ℃ and 15bar pressure, cooled to room temperature, exposed to light in the air for 2 hours, calcined for 2 hours at 550 ℃, washed by deionized water and dried to obtain an adsorbent, wherein the molar ratio of elements of Ca, al, si, na, O and H is as follows: 46:110:360:36:949:1.
Example 2
A method of preparing an adsorbent, the method comprising:
crushing limestone and kaolin, classifying according to the granularity of 2-0.5 mm, selecting 2mm limestone, controlling the concentration of limestone and alkali at 2 g/100 ml, and controlling the mixing time of limestone and alkali at 35 minutes; selecting 0.5mm kaolin, controlling the concentration of the kaolin and alkali at 40 g/100 ml, and controlling the mixing time of the kaolin and alkali at 1.5 hours; the mixture of limestone, kaolin and alkali is reacted in a thermal reactor for 5 minutes at the temperature of 200 ℃ and the pressure of 15bar, cooled to room temperature, exposed to light for 2 hours in the air, calcined for 2 hours at 550 ℃, washed by deionized water and dried to obtain an adsorbent, wherein the molar ratio of elements of Ca, al, si, na, O and H is as follows: 46:110:360:36:949:1.
Example 3
Crushing kaolin, classifying the crushed kaolin according to the granularity of 1-0.5mm, selecting 0.5mm of kaolin, controlling the concentration of the kaolin and alkali to be 38 g/100 ml, and controlling the mixing time of the kaolin and the alkali to be 55 minutes; selecting calcium-silicon slag as a raw material, controlling the concentration of the calcium-silicon slag and alkali at 2 g/100 ml, and controlling the mixing time of the calcium-silicon slag and the alkali at 30 hours; the mixture of the calcium silicon slag, the kaolin and the alkali is reacted in a thermal reactor for 15 minutes at the temperature of 50 ℃ and the pressure of 15bar, is exposed to the air for 2 hours after being cooled to the room temperature, is calcined for 2 hours at 550 ℃, is washed by deionized water and is dried to obtain the adsorbent, and the element mol ratio of Ca to Na to Al to Si to O to H in the final product is 3:1:7:14:44:8.
Example 4
Crushing limestone, classifying according to the granularity of 2-0.5 mm, selecting 2mm limestone, controlling the concentration of limestone and alkali at 2 g/100 ml, and controlling the mixing time of limestone and alkali at 35 minutes; sodium silicon slag is selected as a raw material, the concentration of the sodium silicon slag and alkali is controlled to be 40 g/100 ml, and the mixing time of the sodium silicon slag and the alkali is controlled to be 1.5 hours; the mixture of limestone, sodium silicate slag and alkali is reacted in a thermal reactor for 5 minutes at the temperature of 200 ℃ and the pressure of 15bar, cooled to room temperature, exposed to light in the air for 2 hours, calcined at 550 ℃ for 2 hours, washed by deionized water and dried to obtain the adsorbent, wherein the molar ratio of Ca to Na to Al to Si to O to H in the final product is 3:1:7:14:44:8.
Related experiment and effect data:
the adsorbents prepared in examples 1 to 4 were subjected to elemental composition and percent detection, and the results are shown in the following table:
| calcium% | Aluminium% | Silicon% | Oxygen% | Sodium% | Hydrogen% | |
| Example 1 | 5.95 | 9.61 | 32.62 | 49.13 | 2.68 | 0.0032 |
| Example 2 | 5.95 | 9.61 | 32.62 | 49.13 | 2.68 | 0.0032 |
| Example 3 | 8.36 | 13.16 | 27.30 | 49.03 | 1.60 | 0.557 |
| Example 4 | 8.36 | 13.16 | 27.30 | 49.03 | 1.60 | 0.557 |
Carbon dioxide adsorption performance tests were performed on the adsorbents provided in examples 1 to 4, with specific test conditions: the temperature is 20-25 ℃; test medium: carbon dioxide; test pressure: 1 atmosphere; testing mass of the substance: 14 g; testing carbon dioxide parameters: flow rate 4-5 l/min, concentration: 1200 mg/l. The average values of the test results for the adsorbents provided in examples 1 to 4 are shown in the following table:
carbon dioxide adsorption performance test is carried out on the adsorbents provided in examples 1-4, regeneration is carried out after the test, and specific test conditions in the test process after the regeneration are unchanged, wherein the specific test conditions are as follows: the temperature is 20-25 ℃; test medium: carbon dioxide; test pressure: 1 atmosphere; testing mass of the substance: 14 g; testing carbon dioxide parameters: flow rate 4-5 l/min, concentration: 1200 mg/l. The average values of the results of the carbon dioxide adsorption performance test after the fifth regeneration of the adsorbents provided in examples 1 to 4 are shown in the following table:
| adsorption time (h) | Number of times of regeneration (secondary) | Adsorption quantity (mg/g) (average value) |
| 80 | 5 | 4403 |
| 100 | 5 | 5835 |
| 120 | 5 | 6540 |
| 140 | 5 | 7005 |
| 160 | 5 | 7523 |
| 180 | 5 | 8014 |
| 200 | 5 | 8806 |
The two tables can obtain that the adsorbent provided by the embodiment of the application has better adsorption performance and can still keep higher adsorption capacity after multiple regenerations.
Various embodiments of the present application may exist in a range format; it should be understood that the description in a range format is merely for convenience and brevity and should not be interpreted as a rigid limitation on the scope of the application. It is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In this application, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present application, the terms "include", "comprise", "comprising" and the like mean "including but not limited to".
Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method of preparing an adsorbent, the method comprising:
obtaining particles containing calcium oxide and kaolin;
mixing the calcium oxide component-containing particles, kaolin particles and hydroxyl ion component-containing substances, and performing hydrothermal reaction to obtain an intermediate product;
and cooling the intermediate product, and sintering to obtain the adsorbent.
2. The method for producing an adsorbent according to claim 1, wherein the molded average particle diameter of the calcium oxide-containing component particles is 2 to 4mm; and/or
The average particle diameter of the kaolin particles is 0.4-0.7mm.
3. The method for producing an adsorbent according to claim 1, wherein the mass of the calcium oxide-containing component particles mixed per 100 ml of the hydroxide ion-containing component material is 1 to 2.5g; and/or
The mass of the kaolin particles mixed per 100 ml of the hydroxide ion containing component material is 30-45g.
4. The method for producing an adsorbent according to claim 1, wherein the mixing time of the calcium oxide-containing component particles and the hydroxide ion-containing component substance is 0.5 to 1 hour; and/or
The mixing time of the kaolin particles and the hydroxide ion component containing substance is 1.5h to 2.5h.
5. The method for producing an adsorbent according to claim 1, wherein the temperature of the hydrothermal reaction is 30 to 300 ℃; or (b)
The temperature of the hydrothermal reaction is 50-200 ℃.
6. The method for producing an adsorbent according to claim 1, wherein the cooling is natural cooling; and/or
The cooling time is 1.5-2.5h.
7. The method of producing an adsorbent according to claim 1, wherein the sintering temperature is 400 to 900 ℃; and/or
The sintering time is 1-4h.
8. The method of producing an adsorbent according to claim 7, wherein the sintering temperature is 450 to 550 ℃; and/or
The sintering time is 1.5-2.5h.
9. An adsorbent, characterized in that it is produced by the process for producing an adsorbent according to any one of claims 1 to 8.
10. Use of an adsorbent, characterized in that the use comprises the use of the adsorbent for the absorption of gases, the adsorbent being according to claim 9.
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| CN113856617A (en) * | 2021-10-08 | 2021-12-31 | 山西大学 | Preparation method of calcium-based carbon dioxide adsorbent |
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| CN102815926A (en) * | 2012-08-31 | 2012-12-12 | 南开大学 | High-temperature calcium-based coal ash absorbent for CO2 and preparation method of high-temperature calcium-based coal ash absorbent |
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