CN115069226A - Modified steel slag adsorbent and preparation method and application thereof - Google Patents
Modified steel slag adsorbent and preparation method and application thereof Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 138
- 239000002893 slag Substances 0.000 title claims abstract description 138
- 239000010959 steel Substances 0.000 title claims abstract description 138
- 239000003463 adsorbent Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 23
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000428 dust Substances 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 238000004064 recycling Methods 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010306 acid treatment Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 26
- 238000001179 sorption measurement Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000003546 flue gas Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000002594 sorbent Substances 0.000 claims 1
- 239000002910 solid waste Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000012986 modification Methods 0.000 description 13
- 230000004048 modification Effects 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 11
- 239000011148 porous material Substances 0.000 description 9
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- 238000012216 screening Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
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- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
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- 238000004154 testing of material Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- 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
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Engineering & Computer Science (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The invention discloses a modified steel slag adsorbent, a preparation method and application thereof, wherein the modified steel slag adsorbent is a substrate material of steel slag modified by polyethyleneimine, and the surface of the substrate material is provided with porous SiO 2 Nano hydrophobic coating, noted SiO 2 @ PEIx-Salg, wherein PEI is polyethyleneimine, x is the mass percent of the polyethyleneimine in the steel slag, x =10-30, and Salg represents the steel slag after hydrochloric acid treatment. The invention recycles the resources of the solid waste of the steel slag, the steel slag has the basic characteristics of the adsorbent, and the alkaline reagent and the hydrophobic SiO are adopted 2 The nano particles modify the steel slag and can be used for preparing CO with water resistance and dust resistance 2 Recycling the solid waste of the steel slag while using the adsorbentThe purpose of treating wastes with wastes is realized, and the method has the significance of environmental protection and resource saving.
Description
Technical Field
The invention belongs to the technical field of carbon capture, and particularly relates to a modified steel slag adsorbent and a preparation method and application thereof.
Background
Since the industrial revolution, the combustion of fossil fuels has resulted in a dramatic increase in the carbon dioxide content of the atmosphere from 290PPM prior to the industrial revolution to 400 PPM. In addition to causing global warming, carbon dioxide emissions also pose significant environmental challenges.
Billions of tons of industrial solid wastes are generated in China every year, and the comprehensive utilization rate is only about 50%. The rest solid wastes are accumulated in a centralized way, which not only occupies the land, but also causes the problems of water pollution, soil pollution, air pollution and the like. A large amount of steel slag is inevitably generated in the steel-making process, and the treatment and resource utilization of the steel slag have important significance. Because the steel slag contains various mineral elements, the steel slag is used for replacing limestone to absorb SO in flue gas 2 . The steel slag has the basic characteristics of the adsorbent, such as large specific surface area and developed pore passages. CO 2 2 Is acid gas, and the alkaline adsorbent has good selectivity and adsorption capacity to the acid gas, however, the flue gas after high-efficiency denitration, dust removal and desulfurization contains 10 percent of water vapor and particulate matters (less than or equal to 5 mg/m) 3 ) And the like, the adsorbent is required to have water resistance and dust deposition resistance.
Patent application No. CN201810896849.X discloses a steel slag modification and comprehensive utilization system and method, belongs to the field of metallurgical industry solid waste treatment, and solves the technical problems that a large amount of ferrite compounds in the steel slag cannot be recovered and the steel slag is influenced to serve as a stable building material in the conventional steel slag treatment process of cooling, crushing and magnetic separation. The invention provides a steel slag modification and comprehensive utilization system, which comprises a steel slag modification electric furnace, wherein the modification electric furnace comprises a modification electric furnace main body, an electrode, a first spray pipe and a second spray pipe; the first spray pipe and the second spray pipe are both telescopic structures; the first spray pipe sprays the reducing agent into the modification electric furnace by utilizing the telescopic structure and the compressed gas; the second spray pipe also sprays auxiliary materials into the modification electric furnace by utilizing a telescopic structure. According to the invention, the liquid steel slag is subjected to temperature raising modification treatment by adopting a modification electric furnace, iron oxide in the liquid steel slag is reduced into molten iron, iron components in the steel slag are recovered, and other auxiliary materials are added according to the requirement to perform appropriate quenching and tempering treatment on the steel slag, so that the steel slag components meet the requirement of subsequent recycling.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a modified steel slag adsorbent, a preparation method and application thereof, which are used for improving the resource utilization of steel slag and solving the problem of CO in the prior art 2 Low adsorption and separation efficiency and the like. The specific technical scheme of the invention is as follows:
the modified steel slag adsorbent is a substrate material of steel slag modified by polyethyleneimine, and the surface of the substrate material is provided with porous SiO 2 Nano hydrophobic coating, noted SiO 2 @ PEIx-Salg, wherein PEI is polyethyleneimine, x is the mass percent of the polyethyleneimine in the steel slag, x =10-30, and Salg represents the steel slag after hydrochloric acid treatment.
Further, the porous SiO 2 The thickness of the nano hydrophobic coating is 60-80 nm.
A method for preparing a modified steel slag adsorbent, comprising the steps of:
step 1, weighing 20 g of steel slag, placing the steel slag in a conical flask, and adding 30 mL of 15% HC1 solution for acid washing;
step 2, carrying out suction filtration on the steel slag after acid washing, washing the steel slag with deionized water until the filtrate is neutral, then placing the steel slag in a drying oven for drying, grinding and sieving;
step 3, putting 0.3-0.9g of polyethyleneimine into 30 mL of ethanol, and magnetically stirring for 15 min until the polyethyleneimine is completely dissolved; adding 3g of the steel slag obtained in the step 2, soaking for 6 h, and then placing a sample in a drying oven to obtain a steel slag mark PEIx-Salg modified by polyethyleneimine, wherein x = 10-30;
step 4, taking the polyethyleneimine modified steel slag obtained in the step 3 as a substrate, and spraying hydrophobic SiO by using a spraying method 2 Modifying the nano particles on the substrate to form porous SiO 2 And (5) obtaining a final product by using the nano hydrophobic coating.
The temperature in the drying oven in step 3 was set to 80 ℃.
And (3) fixing the conical flask in a constant-temperature oscillator during acid washing in the step 1, wherein the oscillation time is 1 h.
And (3) grinding the steel slag in the step 2, and screening by using screens of 40 meshes and 60 meshes.
The impregnation process in step 3 is carried out under the conditions of stirring and 50 ℃ water bath.
Step 4, hydrophobic SiO is sprayed before spraying 2 The nano particles are dissolved in gasoline and form SiO along with the volatilization of the gasoline 2 The nano particle mesoporous coating structure has the aperture of 3-5 nm; preferably, the volatile gasoline is recovered by condensation for recycling.
Application of modified steel slag adsorbent in CO of dust-containing water-containing flue gas 2 And (5) adsorption separation.
The invention recycles the resources of the solid waste of the steel slag, utilizes the basic characteristics that the steel slag has higher specific surface area and the steel slag has an adsorbent, adopts an alkaline reagent and hydrophobic SiO 2 The modification of the steel slag by the nano particles and the modification of the steel slag by the alkaline polyethyleneimine are used for preparing the low-cost CO 2 An efficient approach to adsorbents. Aiming at the characteristic that the actual flue gas generally contains impurities such as water vapor, trace particles and the like, mesoporous SiO is sprayed on the surface of the modified steel slag 2 The nano hydrophobic coating can greatly improve the water resistance and the dust deposition resistance of the material. Can be used for preparing CO with water resistance and dust resistance 2 The adsorbent can be used for recycling the solid steel slag waste, so that the purpose of treating waste by waste is realized, and the adsorbent has the significance of environmental protection and resource saving.
Drawings
FIG. 1 is a low-temperature nitrogen adsorption-desorption isotherm of steel slag and modified steel slag provided in the blank examples and examples 1 to 3 of the present invention;
FIG. 2 is the low temperature nitrogen adsorption and desorption isotherms of the steel slag and the modified steel slag provided in the blank example and comparative examples 1 to 3;
FIG. 3 shows the steel slag and modified steel slag CO 2 Adsorption amount, absorption amount, and dust absorption amount. a-Salg-raw, b-PEI 10 -Salg;c-PEI 20 -Salg;d-PEI 30 -Salg;e-SiO 2 @PEI 10 -Salg;f-SiO 2 @PEI 20 -Salg; g-SiO 2 @PEI 30 -Salg。
Detailed Description
The invention is further described below with reference to the accompanying drawings and specific embodiments.
Example 1
Firstly, weighing 20 g of steel slag, placing the steel slag in a conical flask, adding 30 mL of 15% HC1 solution, fixing the conical flask in a constant-temperature oscillator, and oscillating and acid-washing for 1 h to remove easily soluble substances;
then, filtering the steel slag after acid washing, repeatedly washing the steel slag with deionized water for many times until the filtrate is neutral, then placing the steel slag in a drying oven for overnight drying at 80 ℃, and screening the steel slag by using screens of 40 meshes and 60 meshes after grinding for later use;
then, 0.3g of polyethyleneimine PEI is placed in 30 mL of ethanol, and magnetic stirring is carried out for 15 min until complete dissolution is achieved; adding 3g of steel slag, and soaking for 6 hours under the conditions of stirring and 50 ℃ water bath; putting the sample in a drying oven, and drying at 80 ℃ overnight to obtain the steel slag label modified by the polyethyleneimine as PEI 10 -Salg；
Finally, taking the modified steel slag as a substrate, and adding hydrophobic SiO 2 Dissolving the nano particles in gasoline, spraying the solution on a substrate, and volatilizing the gasoline to form porous SiO 2 Nano hydrophobic coating, sample label is SiO 2 @PEI 10 Salg, recovery of the volatile gasoline by condensation for recycling.
Example 2
Firstly, weighing 20 g of steel slag, placing the steel slag in a conical flask, adding 30 mL of 15% HC1 solution, fixing the conical flask in a constant-temperature oscillator, and oscillating and acid-washing for 1 h to remove easily soluble substances;
then, filtering the steel slag after acid washing, repeatedly washing the steel slag with deionized water for many times until the filtrate is neutral, then placing the steel slag in a drying oven for overnight drying at 80 ℃, and screening the steel slag by using screens of 40 meshes and 60 meshes after grinding for later use;
then, 0.6g of Polyethyleneimine (PEI) was placed in 30 mL of ethanol and magnetically stirred for 15 min until complete dissolution; adding 3g of steel slag, and soaking for 6 hours under the conditions of stirring and 50 ℃ water bath; putting the sample in a drying oven, and drying at 80 ℃ overnight to obtain a steel slag label modified by polyethyleneimine, namely PEI 20-Salg;
finally, taking the modified steel slag as a substrate, and adding hydrophobic SiO 2 Dissolving the nano particles in gasoline, spraying the solution on a substrate, and volatilizing the gasoline to form porous SiO 2 Nano hydrophobic coating, sample label is SiO 2 @PEI 20 Salg, volatile gasoline is recovered by condensation in the process for recycling.
Example 3
Firstly, weighing 20 g of steel slag, placing the steel slag in a conical flask, adding 30 mL of 15% HC1 solution, fixing the conical flask in a constant-temperature oscillator, and oscillating and acid-washing for 1 h to remove easily soluble substances;
then, filtering the steel slag after acid washing, repeatedly washing the steel slag with deionized water for many times until the filtrate is neutral, then placing the steel slag in a drying oven for overnight drying at 80 ℃, and screening the steel slag by using screens of 40 meshes and 60 meshes after grinding for later use;
then, 0.9g of polyethyleneimine PEI is placed in 30 mL of ethanol, and magnetic stirring is carried out for 15 min until complete dissolution is achieved; adding 3g of steel slag, and soaking for 6 hours under the conditions of stirring and 50 ℃ water bath; putting the sample in a drying oven, and drying at 80 ℃ overnight to obtain the steel slag label modified by the polyethyleneimine as PEI 30 -Salg；
Finally, taking the modified steel slag as a substrate, and adding hydrophobic SiO 2 Dissolving the nano particles in gasoline, spraying the solution on a substrate, and volatilizing the gasoline to form porous SiO 2 Nano hydrophobic coating, sample label is SiO 2 @PEI 30 Salg, volatile gasoline is recovered by condensation in the process for recycling.
Comparative example 1
Firstly, weighing 20 g of steel slag, placing the steel slag in a conical flask, adding 30 mL of 15% HC1 solution, fixing the conical flask in a constant-temperature oscillator, and oscillating and acid-washing for 1 h to remove easily soluble substances;
then, filtering the steel slag after acid washing, repeatedly washing the steel slag with deionized water for many times until the filtrate is neutral, then placing the steel slag in a drying oven for overnight drying at 80 ℃, and screening the steel slag by using screens of 40 meshes and 60 meshes after grinding for later use;
finally, 0.3g of polyethyleneimine PEI was placed in 30 mL of EtOHIn alcohol, magnetically stirring for 15 min until completely dissolving; adding 3g of steel slag, and soaking for 6 hours under the conditions of stirring and 50 ℃ water bath; putting the sample in a drying oven, and drying at 80 ℃ overnight to obtain the steel slag label modified by the polyethyleneimine as PEI 10 -Salg。
Comparative example 2
Firstly, weighing 20 g of steel slag, placing the steel slag in a conical flask, adding 30 mL of 15% HC1 solution, fixing the conical flask in a constant-temperature oscillator, and oscillating and acid-washing for 1 h to remove easily soluble substances;
then, carrying out suction filtration on the steel slag after acid washing, repeatedly washing the steel slag with deionized water for many times until filtrate is neutral, then placing the steel slag in a drying oven for overnight drying at 80 ℃, and screening the steel slag with screens of 40 meshes and 60 meshes for later use after grinding;
finally, 0.6g of polyethyleneimine PEI is placed in 30 mL of ethanol, and magnetic stirring is carried out for 15 min until complete dissolution is achieved; adding 3g of steel slag, and soaking for 6 hours under the conditions of stirring and 50 ℃ water bath; putting the sample in a drying oven, and drying at 80 ℃ overnight to obtain the steel slag label modified by the polyethyleneimine as PEI 20 -Salg。
Comparative example 3
Firstly, weighing 20 g of steel slag, placing the steel slag in a conical flask, adding 30 mL of 15% HC1 solution, fixing the conical flask in a constant-temperature oscillator, and oscillating and acid-washing for 1 h to remove easily soluble substances;
then, carrying out suction filtration on the steel slag after acid washing, repeatedly washing the steel slag with deionized water for many times until filtrate is neutral, then placing the steel slag in a drying oven for overnight drying at 80 ℃, and screening the steel slag with screens of 40 meshes and 60 meshes for later use after grinding;
finally, 0.9g of polyethyleneimine PEI is placed in 30 mL of ethanol, and magnetic stirring is carried out for 15 min until complete dissolution is achieved; adding 3g of steel slag, and soaking for 6 hours under the conditions of stirring and 50 ℃ water bath; putting the sample in a drying oven, and drying at 80 ℃ overnight to obtain the steel slag label modified by the polyethyleneimine as PEI 30 -Salg。
And testing the specific surface area and the pore volume of the steel slag and the modified steel slag by adopting a specific surface area and pore diameter analyzer. Testing the material in dry and dustless condition by using U-shaped tube adsorberCO of 2 Dynamic adsorption quantity Q1, intake air is N 2 /CO 2 (15% volume fraction CO) 2 ) Mixing gas, adsorbing at 60 deg.C, controlling temperature with water bath, and detecting CO with gas chromatography 2 Concentration, calculating the adsorption amount according to the peak area; testing of materials for CO at the same temperature under conditions of moisture and particulate matter 2 Dynamic adsorption capacity Q 2 Talc powder is used to simulate particles; in addition, the adsorption amount of the material to the single component of water vapor and particulate matter at 60 ℃ is respectively tested, and the adsorption amount and the dust absorption amount are calculated by adopting a gravimetric method. The low-temperature nitrogen adsorption and desorption isotherms are shown in fig. 1-2, the steel slag and the modified steel slag both show a typical IV-type isotherm and show an H2-type hysteresis loop, which indicates that the sample is a mesoporous material with uniform pore size distribution and the pore structure is an ink bottle type. Specific surface area of adsorbent, pore volume, CO 2 The results of the adsorption, absorption and dust absorption measurements are shown in Table 1, and the CO contents of the different samples 2 The change law of the adsorption amount, the absorption amount and the dust absorption amount is shown in fig. 3.
TABLE 1 specific surface area of adsorbent, pore volume, CO 2 Adsorption amount, absorption amount and dust collection amount
As can be seen from Table 1, the Salg-raw has a specific surface area of 284 m 2 Per g, pore volume 0.65 m 3 G, dry, dustless CO 2 The adsorption quantity Q1 is 70 mg/g, after modification by PEI, the specific surface area and pore volume of the steel slag are gradually reduced along with the increase of the organic amine loading quantity, and CO 2 The adsorption quantity Q1 is gradually increased along with the increase of the loading quantity, and PEI 30 Salg gave the highest adsorption capacity, 135.1 mg/g; salg-raw and PEI 30 CO of Salg under dusty, hydrous conditions 2 The adsorption amount Q2 decreased to 48.3 mg/g and 98.4mg/g, respectively. After the PEI is adopted for modification, the water absorption capacity and the dust absorption capacity of the steel slag are increased along with the increase of the amine loading capacity, and the water resistance and the dust resistance of the amine modified steel slag are reduced due to the hydrophilicity and the adhesion of the PEI.
Compared with PEIx-Salg, porous SiO is adopted 2 Sample SiO modified by nano hydrophobic coating 2 @ PEIx-Salg CO 2 The adsorption quantity Q1 slightly decreases, while CO 2 The adsorption capacity Q2 was significantly increased, and the water absorption capacity and dust collection capacity were significantly reduced. Thus, SiO 2 The @ PEIx-Salg adsorbent has good water and dust resistance, and is suitable for CO under complex working conditions 2 And (5) adsorption separation.
Claims (10)
1. The modified steel slag adsorbent is characterized in that the steel slag modified by polyethyleneimine is used as a substrate material, and the surface of the substrate material is provided with porous SiO 2 Nano hydrophobic coating, noted SiO 2 @ PEIx-Salg, wherein PEI is polyethyleneimine, x is the mass percent of the polyethyleneimine in the steel slag, x =10-30, and Salg represents the steel slag after hydrochloric acid treatment.
2. The modified steel slag sorbent of claim 1, wherein the porous SiO is 2 The thickness of the nano hydrophobic coating is 60-80 nm.
3. A method of preparing the modified steel slag adsorbent of claim 1 or 2, characterized by comprising the steps of:
step 1, weighing 20 g of steel slag, placing the steel slag in a conical flask, and adding 30 mL of 15% HC1 solution for acid washing;
step 2, carrying out suction filtration on the steel slag after acid washing, washing the steel slag with deionized water until the filtrate is neutral, then placing the steel slag in a drying oven for drying, grinding and sieving;
step 3, putting 0.3-0.9g of polyethyleneimine into 30 mL of ethanol, and magnetically stirring for 15 min until the polyethyleneimine is completely dissolved; adding 3g of the steel slag obtained in the step 2, soaking for 6 h, and then placing a sample in a drying oven to obtain a steel slag mark PEIx-Salg modified by polyethyleneimine, wherein x = 10-30;
step 4, taking the polyethyleneimine modified steel slag obtained in the step 3 as a substrate, and spraying hydrophobic SiO by using a spraying method 2 Modifying the nano particles on the substrate to form porous SiO 2 Nano-scale dredgeAnd (5) coating with water to obtain a final product.
4. The method for preparing the modified steel slag adsorbent according to claim 3, wherein the temperature in the drying oven in the step 3 is set to 80 ℃.
5. The method for preparing the modified steel slag adsorbent according to claim 3, wherein the conical flask is fixed in a constant temperature oscillator for 1 h during the acid washing in the step 1.
6. The method for preparing the modified steel slag adsorbent according to claim 3, wherein the steel slag is ground in the step 2 and then screened by using 40-mesh and 60-mesh screens.
7. The method for preparing the modified steel slag adsorbent according to claim 3, wherein the impregnation process in the step 3 is performed under the conditions of stirring and 50 ℃ water bath.
8. The method for preparing the modified steel slag adsorbent according to claim 3, characterized in that the hydrophobic SiO is sprayed before the spraying in step 4 2 The nano particles are dissolved in gasoline and form SiO along with the volatilization of the gasoline 2 The nano particle mesoporous coating structure has the aperture of 3-5 nm.
9. The method for preparing the modified steel slag adsorbent according to claim 8, wherein the volatile gasoline is recovered by a condensation method for recycling.
10. Use of the modified steel slag adsorbent as claimed in claim 1 or 2 for CO in flue gas containing dust and water 2 And (5) adsorption separation.
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