CN112742349A - For CO2Trapped magnetic ionic liquid nano composite adsorption material - Google Patents
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 88
- 239000000463 material Substances 0.000 title claims abstract description 57
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 35
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000696 magnetic material Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 50
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000007885 magnetic separation Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 16
- 239000012265 solid product Substances 0.000 claims description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 13
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 claims description 13
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 11
- 239000004094 surface-active agent Substances 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- WSSMOXHYUFMBLS-UHFFFAOYSA-L iron dichloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Fe+2] WSSMOXHYUFMBLS-UHFFFAOYSA-L 0.000 claims description 9
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- -1 amine salt cation Chemical class 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- 150000001413 amino acids Chemical group 0.000 claims description 4
- 150000001450 anions Chemical class 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- HDMXIELEUKTYFR-UHFFFAOYSA-N bis(2-ethylhexyl) butanedioate;sodium Chemical compound [Na].CCCCC(CC)COC(=O)CCC(=O)OCC(CC)CCCC HDMXIELEUKTYFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 239000003093 cationic surfactant Substances 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- WCVHUIPWSPEOIG-UHFFFAOYSA-N n,n-dimethylheptadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCN(C)C WCVHUIPWSPEOIG-UHFFFAOYSA-N 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 39
- 239000003463 adsorbent Substances 0.000 abstract description 20
- 125000003368 amide group Chemical group 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 229910002090 carbon oxide Inorganic materials 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 33
- 239000000243 solution Substances 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000001569 carbon dioxide Substances 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 9
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 7
- 229920006395 saturated elastomer Polymers 0.000 description 7
- 238000002411 thermogravimetry Methods 0.000 description 7
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 3
- 229920000053 polysorbate 80 Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-M Aminoacetate Chemical compound NCC([O-])=O DHMQDGOQFOQNFH-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 description 1
- 239000013504 Triton X-100 Substances 0.000 description 1
- 229920004890 Triton X-100 Polymers 0.000 description 1
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- JMJRNNLOJLYQLM-UHFFFAOYSA-N azane;propan-1-ol Chemical compound N.CCCO JMJRNNLOJLYQLM-UHFFFAOYSA-N 0.000 description 1
- GKFQZRDNTUZMKS-JEDNCBNOSA-N butan-1-amine;(2s)-2,6-diaminohexanoic acid Chemical compound CCCCN.NCCCC[C@H](N)C(O)=O GKFQZRDNTUZMKS-JEDNCBNOSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001412 inorganic anion Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229940071089 sarcosinate Drugs 0.000 description 1
- FSYKKLYZXJSNPZ-UHFFFAOYSA-N sarcosine Chemical compound C[NH2+]CC([O-])=O FSYKKLYZXJSNPZ-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
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- 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
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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Abstract
The invention provides a method for preparing CO2And (3) the trapped magnetic ionic liquid nano composite adsorption material. The invention loads the amido-containing ionic liquid on the surface of a nano magnetic material carrier to form the carrier for capturing CO2The amido ionic liquid can adsorb CO with high capacity2The loss is less, the specific surface area and the dispersity of the nano material can be remarkably improved, so that the adsorption capacity is improved, and the magnetic material can realize the quick and efficient recovery of the adsorbent by utilizing a magnetic field. The invention has high adsorption capacity, strong stability, no loss of ionic liquid and larger CO at higher temperature2Capacity and the adsorbent can be quickly and efficiently recovered, so thatThe method has good prospect in the field of carbon oxide capture.
Description
Technical Field
The invention belongs to the technical field of carbon dioxide capture, and relates to a method for capturing carbon dioxide in a gas source by an adsorption method, which realizes high-capacity, low-energy-consumption and recyclable capture of the carbon dioxide.
Background
Excessive emissions of carbon dioxide have serious negative impacts on the global climate environment. The control of carbon dioxide emission is directly related to industrial production, climate, human health and energy conservation, so the research on carbon dioxide capture technology is very important and urgent.
CO2The trapping technique of (2) includes a solvent absorption method, an adsorption method, a low-temperature separation method, a membrane separation method and the like. CO capture and separation by adsorption2Low energy consumption, low investment and trapping operation cost and the like, and is considered as a very promising CO2A trapping technique.
A good adsorbent is CO2The key points of the trapping and separation are as follows: large adsorption capacity, good selectivity, good regeneration performance, high adsorption rate, good thermal stability, good mechanical strength and the like.
Because the common adsorbent (active carbon and other porous carbon-based and silicon-based materials) has poor adsorption quantity and selectivity, and the adsorbent is used for trapping CO2The loss of the adsorbent is easily caused by the loss of the air flow in the process. The magnetic material is used as the adsorption material of the carrier, so that the adsorption material is easy to recycle due to the magnetism, and the problem of loss of the adsorbent can be preferentially avoided.
The ionic liquid is a molten salt system which is composed of specific organic cations and organic or inorganic anions and is in a liquid state at room temperature or near room temperature, has the advantages of good stability, low volatility, strong carbon dioxide dissolving capacity, designability and the like, and has great application potential in the aspect of carbon dioxide capture.
But because the ionic liquid is expensive at presentAnd the viscosity is high, so that the large-scale application of the ionic liquid is prevented. Thus, ionic liquid loading and carrier application to CO2The adsorption has the advantages of absorption and adsorption, and becomes a way for solving the problem of large-scale application of the existing ionic liquid.
Disclosure of Invention
The invention provides a method for preparing CO2And (3) the trapped magnetic ionic liquid nano composite adsorption material.
The above object of the present invention is achieved by the following technical solutions: for CO2The trapped magnetic ionic liquid nano composite adsorption material is a composite material in which an amido-containing ionic liquid is loaded on the surface of a nano magnetic material carrier.
In general, the invention is described for use with CO2The trapped magnetic ionic liquid nano composite adsorbing material has the loaded ionic liquid content of 20-90 wt%, and preferably has the loaded ionic liquid content of 40-70 wt%; the nano magnetic material is Fe3O4-SiO2。
The invention also provides a method for CO2The preparation method of the trapped magnetic ionic liquid nano composite adsorption material comprises the following steps:
step 1: FeCl3.6H2O and FeCl2.4H2O is added to [ Bmim ] under nitrogen protection]Stirring and fully mixing the solution in Cl, then gradually dropwise adding concentrated ammonia water into the system for reaction, and reacting the ammonia water with reactants in the solution layer to generate Fe3O4，Fe3O4Washing, magnetically separating and drying to obtain powdered Fe3O4Particles;
step 2: dissolving surfactant in hydrochloric acid at room temperature, adjusting pH to 1-5, adding mesitylene and ammonium fluoride, heating the mixture to 37-38 deg.C under stirring, maintaining for more than 30min, and adding powdered Fe3O4Adding the particles and the silicon source compound into the mixture, heating the mixture to the temperature of 100-120 ℃, maintaining the temperature for 20-22h, cooling the mixture to room temperature, performing magnetic separation to obtain a solid product, washing, performing magnetic separation, drying, and calcining the solid product at the temperature of 400-450 ℃ for more than 8 hours;
and step 3: dissolving the ionic liquid in ethanol, dispersing the carrier obtained in the step 2 in the ethanol solution of the ionic liquid, stirring for 8-10 hours at 20-50 ℃, washing, carrying out magnetic separation, drying to obtain powdery particles, removing ethanol, and drying at 50-60 ℃ to obtain the magnetic ionic liquid composite adsorbing material.
Preferably, step 1: FeCl3.6H2O and FeCl2.4H2O is added to [ Bmim ] under nitrogen protection]Mechanically stirring and fully mixing in Cl, gradually dripping concentrated ammonia water into the system to react for 30min after the temperature is stabilized at 70 ℃, and reacting ammonia water serving as a precipitator with reactants in a solution layer to generate Fe3O4，Fe3O4Washing with 50% ethanol water solution and deionized water for several times, magnetically separating, and vacuum drying to obtain powder particles;
preferably, step 2: dissolving surfactant in hydrochloric acid at room temperature, adjusting pH to 1-5, adding mesitylene and ammonium fluoride, heating the mixture to 37-38 deg.C under stirring, maintaining for more than 30min, and adding Fe3O4Adding the particles and the silicon source compound into the mixture, heating the mixture to the temperature of 100-120 ℃, maintaining the temperature for 20-22h, cooling the mixture to room temperature, carrying out magnetic separation to obtain a solid product, washing the solid product for a plurality of times by using a 50% ethanol aqueous solution and deionized water, carrying out magnetic separation, drying the solid product in air, and calcining the solid product for more than 8 hours at the temperature of 400-450 ℃;
preferably, step 3: dissolving the ionic liquid in ethanol, dispersing the carrier obtained in the step 2 in an ethanol solution of the ionic liquid, stirring for 8-10 hours at 20-50 ℃, washing with a 50% ethanol aqueous solution and deionized water for a plurality of times, performing magnetic separation, performing vacuum drying to obtain powdery particles, heating or vacuumizing to remove ethanol, and drying at 50-60 ℃ to obtain the ionic liquid adsorbing material.
Preferably, the cation of the ionic liquid is one or more of organic amine salt cation and organic alcohol amine cation.
The anion of the ionic liquid is an anion with an amino acid structure, and the structural formula of the amino acid is H2N-R-COOH(R＝CnH2n，n ＝1～5) 。
The surfactant can be nonionic surfactant pan80, tween series; the cationic surfactant is sodium bis (2-ethylhexyl) succinate sulfonate, hexadecyl trimethyl ammonium bromide, hexadecyl trimethyl amine, etc.; the anionic surfactant is sodium lauryl sulfate, etc.
The surfactant may be one or more of the above surfactants.
The silicon source compound is ethyl silicate, sodium silicate and NaHSi2O5.3H2One or more of O.
The mass ratio of the surfactant to the mesitylene is 2: 1-1: 4.
The mass ratio of the silicon source compound to the surfactant is 3: 1-1: 3.
The invention is used for CO2The trapped magnetic ionic liquid nano composite adsorption material is suitable for CO2The partial pressure is 5kPa-1 MPa.
In general, CO is adsorbed2The temperature is 30-130 ℃.
The invention loads the amido-containing ionic liquid on the surface of a nano magnetic material carrier to form the carrier for capturing CO2The amido ionic liquid can adsorb CO with high capacity2The loss is less, the specific surface area and the dispersity of the nano material can be remarkably improved, so that the adsorption capacity is improved, and the magnetic material can realize the quick and efficient recovery of the adsorbent by utilizing a magnetic field.
The invention provides a method for CO2The trapped magnetic ionic liquid nano composite adsorption material has high adsorption capacity, strong stability, no loss of ionic liquid and larger CO at higher temperature2Capacity and the adsorbent can be quickly and efficiently recovered, and the like, so the method has good prospect in the field of carbon dioxide capture.
Drawings
Fig. 1 is a TEM photograph of the composite adsorbent in example 1 of the present invention.
Fig. 2 is a schematic view showing that the adsorbent having adsorbed carbon dioxide in example 1 was recovered by a magnet.
Detailed Description
The present invention is illustrated by the following examples, but the present invention is not limited to the following examples. Variations and implementations are included in the technical scope of the present invention without departing from the spirit of the invention described above and below.
Example 1
1.148molFeCl3.6H2O with 0.574mol FeCl2.4H2O is added to 2.296mol [ Bmim ] under the protection of nitrogen]In Cl, mix well with mechanical stirring. After the temperature is stabilized at 70 ℃, 400ml of concentrated ammonia water is gradually dripped into the system. Fe3O4Washing with 50% ethanol water solution and deionized water for several times, magnetically separating, and vacuum drying to obtain powder.
10g of pan80 were dissolved in 1.0M hydrochloric acid at room temperature, 50 g of mesitylene and 100 mg of ammonium fluoride were added thereto, and the mixture was heated to 37 ℃ with stirring for 30 min. 30g of ethyl silicate and 20g of Fe3O4Added thereto and heated to 100 ℃ for 20h, the mixture was cooled to room temperature, magnetically separated to give a solid product and dried in air and calcined at 400 ℃ for 16 h.
Dispersing a certain amount of tetramethylammonium hydroxide glycinate ionic liquid and a carrier in an ethanol solution according to the mass ratio of 1:3, and stirring for 16 hours at 20 ℃. Heating or vacuumizing to remove ethanol, and drying at 60 ℃ to obtain the ionic liquid magnetic adsorption material.
The microstructure of the adsorbent material was characterized by projection electron microscopy (TEM) as shown in figure 1.
The ionic liquid content and the material stability in the adsorbent material were investigated by thermogravimetric analysis (TGA/DTA).
The material is firstly N2(100%) heating to 110 ℃ under atmosphere to remove free water and pre-adsorbed CO2. Then in air (40%) and N2(60%) in a mixed atmosphere, the mixture was heated to 1000 ℃ at a heating rate of 10 ℃ per min. The ionic liquid content was 41wt% as calculated from the change in sample mass over a temperature range of 150 ℃ to 1000 ℃. The initial decomposition temperature of the ionic liquid is 380 ℃.
Adsorbing CO by using ionic liquid adsorbing material at 1MPa and 30 DEG C2The saturated adsorption capacity after reaching equilibrium was 139.4 mg/g.
The magnetic ionic liquid adsorbent having adsorbed carbon dioxide was recovered by a magnet as shown in fig. 2.
Example 2
1.148molFeCl3.6H2O with 0.574mol FeCl2.4H2O is added to 2.296mol [ Bmim ] under the protection of nitrogen]In Cl, mix well with mechanical stirring. After the temperature is stabilized at 70 ℃, 400ml of concentrated ammonia water is gradually dripped into the system. Fe3O4Washing with 50% ethanol water solution and deionized water for several times, magnetically separating, and vacuum drying to obtain powder.
10g of tween80 were dissolved in 0.8M hydrochloric acid at room temperature, 20g of mesitylene and 200 mg of ammonium fluoride were added thereto, and the mixture was heated to 40 ℃ with stirring for 60 min. 40g of ethyl silicate and 30g of Fe3O4 were added and heated to 100 ℃ for 24h, the mixture was cooled to room temperature, the solid product was isolated magnetically and dried in air and calcined at 420 ℃ for 8 h.
Dispersing a certain amount of n-butylammonium lysine salt ionic liquid and a carrier in an ethanol solution according to a mass ratio of 6:1, and stirring for 8 hours at 30 ℃. Heating or vacuumizing to remove ethanol, and drying at 50 ℃ to obtain the ionic liquid adsorbing material.
The ionic liquid content and the material stability in the adsorbent material were investigated by thermogravimetric analysis (TGA/DTA). The material is firstly N2(100%) heating to 110 ℃ under atmosphere to remove free water and pre-adsorbed CO2. Then in air (40%) and N2(60%) in a mixed atmosphere, the mixture was heated to 1000 ℃ at a heating rate of 10 ℃ per min. The content of the ionic liquid is 80wt% calculated by the change of the sample mass in the temperature range of 150 ℃ to 1000 ℃. The initial decomposition temperature of the ionic liquid is 393 ℃.
The ionic liquid adsorbing material adsorbs CO2 at 5kPa and 80 ℃, and the saturated adsorption capacity is 100.3mg/g after the equilibrium is reached.
Example 3
1.148mol of FeCl3.6H2O and 0.574mol of FeCl2.4H2O are added into 2.296mol of [ Bmim ] Cl under the protection of nitrogen, and the mixture is stirred mechanically and mixed fully. After the temperature is stabilized at 70 ℃, 400ml of concentrated ammonia water is gradually dripped into the system. And washing Fe3O4 with 50% ethanol water solution and deionized water for several times, performing magnetic separation, and vacuum drying to obtain powdery particles.
20g of sodium bis (2-ethylhexyl) succinate sulfonate were dissolved in 0.001M hydrochloric acid at room temperature, 10g of mesitylene and 150 mg of ammonium fluoride were added thereto, and the mixture was heated to 38 ℃ with stirring for 90 min. 30g of NaHSi2O5.3H2O and 25g of Fe3O4 were added thereto and heated to 120 ℃ for 22 hours, the mixture was cooled to room temperature, and the solid product was obtained by magnetic separation, dried in air and calcined at 450 ℃ for 8 hours.
Dispersing a certain amount of tetrahexylammonium hydroxide threonine salt ionic liquid and a carrier in an ethanol solution according to a mass ratio of 4:1, and stirring for 8 hours at 50 ℃. Heating or vacuumizing to remove ethanol, and drying at 30 ℃ to obtain the ionic liquid adsorbing material.
The ionic liquid content and the material stability in the adsorbent material were investigated by thermogravimetric analysis (TGA/DTA). The material was first heated to 110 ℃ under an atmosphere of N2 (100%) to remove free water and pre-adsorbed CO 2. Then, the mixture was heated to 1000 ℃ at a heating rate of 10 ℃ per min under a mixed atmosphere of air (40%) and N2 (60%). The ionic liquid content was calculated from the change in mass of the sample over a temperature range of 150 ℃ to 1000 ℃ and was 53 wt%. The initial decomposition temperature of the ionic liquid is 370 ℃.
The ionic liquid adsorbing material adsorbs CO2 at 100kPa and 120 ℃, and the saturated adsorption capacity is 90.4mg/g after the equilibrium is reached.
Example 4
1.148mol of FeCl3.6H2O and 0.574mol of FeCl2.4H2O are added into 2.296mol of [ Bmim ] Cl under the protection of nitrogen, and the mixture is stirred mechanically and mixed fully. After the temperature is stabilized at 70 ℃, 400ml of concentrated ammonia water is gradually dripped into the system. And washing Fe3O4 with 50% ethanol water solution and deionized water for several times, performing magnetic separation, and vacuum drying to obtain powdery particles.
15 g of cetyltrimethylammonium chloride were dissolved in 0.5M hydrochloric acid at room temperature, 40g of mesitylene and 120 mg of ammonium fluoride were added thereto, and the mixture was heated to 37 ℃ with stirring for 120 min. 5g NaHSi2O5.3H2O and 10g Fe3O4 were added and heated to 100 ℃ for 22h, the mixture was cooled to room temperature, the solid product was obtained by magnetic separation and dried in air and calcined at 400 ℃ for 12 h.
Dispersing a certain amount of n-propanol ammonium sarcosinate ionic liquid and a carrier in an ethanol solution according to a mass ratio of 5:1, and stirring for 8 hours at 50 ℃. Heating or vacuumizing to remove ethanol, and drying at 30 ℃ to obtain the ionic liquid adsorbing material.
The ionic liquid content and the material stability in the adsorbent material were investigated by thermogravimetric analysis (TGA/DTA). The material was first heated to 110 ℃ under an atmosphere of N2 (100%) to remove free water and pre-adsorbed CO 2. Then, the mixture was heated to 1000 ℃ at a heating rate of 10 ℃ per min under a mixed atmosphere of air (40%) and N2 (60%). The ionic liquid content was 73wt% as calculated from the change in sample mass over a temperature range of 150 ℃ to 1000 ℃. The initial decomposition temperature of the ionic liquid is 373 ℃.
The ionic liquid adsorbing material adsorbs CO2 at 130 ℃ under 30kPa, and the saturated adsorption capacity is 87.7mg/g after the equilibrium is reached.
Example 5
1.148mol of FeCl3.6H2O and 0.574mol of FeCl2.4H2O are added into 2.296mol of [ Bmim ] Cl under the protection of nitrogen, and the mixture is stirred mechanically and mixed fully. After the temperature is stabilized at 70 ℃, 400ml of concentrated ammonia water is gradually dripped into the system. And washing Fe3O4 with 50% ethanol water solution and deionized water for several times, performing magnetic separation, and vacuum drying to obtain powdery particles.
20g of sodium dodecyl sulfate were dissolved in 0.02M hydrochloric acid at room temperature, 20g of mesitylene and 200 mg of ammonium fluoride were added thereto, and the mixture was heated to 40 ℃ with stirring for 120 min. 20g of sodium silicate and 40g of Fe3O4 were added and heated to 100 ℃ for 24h, the mixture was cooled to room temperature, the solid product was obtained by magnetic separation and dried in air and calcined at 400 ℃ for 12 h.
Dispersing a certain amount of tetraethylammonium hydroxide valine ionic liquid and a carrier in an ethanol solution according to a mass ratio of 2:1, and stirring for 8 hours at 50 ℃. Heating or vacuumizing to remove ethanol, and drying at 50 ℃ to obtain the ionic liquid adsorbing material.
The ionic liquid content and the material stability in the adsorbent material were investigated by thermogravimetric analysis (TGA/DTA). The material was first heated to 110 ℃ under an atmosphere of N2 (100%) to remove free water and pre-adsorbed CO 2. Then, the mixture was heated to 1000 ℃ at a heating rate of 10 ℃ per min under a mixed atmosphere of air (40%) and N2 (60%). The content of the ionic liquid is 50wt% calculated by the change of the sample mass in the temperature range of 150 ℃ to 1000 ℃. The initial decomposition temperature of the ionic liquid is 366 ℃.
The ionic liquid adsorbing material adsorbs CO2 at 105 ℃ under 15kPa, and the saturated adsorption capacity is 68.7mg/g after the equilibrium is reached.
Example 6
1.148mol of FeCl3.6H2O and 0.574mol of FeCl2.4H2O are added into 2.296mol of [ Bmim ] Cl under the protection of nitrogen, and the mixture is stirred mechanically and mixed fully. After the temperature is stabilized at 70 ℃, 400ml of concentrated ammonia water is gradually dripped into the system. And washing Fe3O4 with 50% ethanol water solution and deionized water for several times, performing magnetic separation, and vacuum drying to obtain powdery particles.
10g Triton X-100, 10g cetyltrimethylammonium bromide were dissolved in 0.02M hydrochloric acid at room temperature, 20g mesitylene and 200 mg ammonium fluoride were added thereto, and the mixture was heated to 40 ℃ with stirring for 120 min. 20g of ethyl silicate and 10g of Fe3O4 were added thereto and heated to 100 ℃ for 24h, the mixture was cooled to room temperature, magnetically separated to give a solid product and dried in air and calcined at 400 ℃ for 12 h.
Dispersing a certain amount of n-hexylammonium alanine salt ionic liquid and a carrier in an ethanol solution according to the mass ratio of 3:1, and stirring for 8 hours at 50 ℃. Heating or vacuumizing to remove ethanol, and drying at 50 ℃ to obtain the ionic liquid adsorbing material.
The ionic liquid content and the material stability in the adsorbent material were investigated by thermogravimetric analysis (TGA/DTA). The material was first heated to 110 ℃ under an atmosphere of N2 (100%) to remove free water and pre-adsorbed CO 2. Then, the mixture was heated to 1000 ℃ at a heating rate of 10 ℃ per min under a mixed atmosphere of air (40%) and N2 (60%). The ionic liquid content was calculated as 71wt% from the change in sample mass over a temperature range of 150 ℃ to 1000 ℃. The initial decomposition temperature of the ionic liquid is 375 ℃.
Adsorbing CO2 on the ionic liquid adsorbing material at 100 ℃ under 15kPa, wherein the saturated adsorption capacity is 79.6mg/g after the equilibrium is reached.
Example 7
1.148mol FeCl3.6H2O and 0.574mol FeCl24H2O was added under nitrogen blanketing to 2.296mol [ Bmim ]]In Cl, mix well with mechanical stirring. After the temperature is stabilized at 70 ℃, 400ml of concentrated ammonia water is gradually dripped into the system. And washing Fe3O4 with 50% ethanol water solution and deionized water for several times, performing magnetic separation, and vacuum drying to obtain powdery particles.
20g of tween80 were dissolved in 0.001M hydrochloric acid at room temperature, 10g of mesitylene and 150 mg of ammonium fluoride were added thereto, and the mixture was heated to 37 ℃ with stirring for 90 min. 30g of sodium silicate and 10g of Fe3O4 were added and heated to 120 ℃ for 24h, the mixture was cooled to room temperature, the solid product was obtained by magnetic separation and dried in air and calcined at 450 ℃ for 8 h.
Dispersing a certain amount of tetrahexylammonium hydroxide threonine salt ionic liquid and a carrier in an ethanol solution according to a mass ratio of 4:1, and stirring for 8 hours at 50 ℃. Heating or vacuumizing to remove ethanol, and drying at 30 ℃ to obtain the ionic liquid adsorbing material.
The ionic liquid content and the material stability in the adsorbent material were investigated by thermogravimetric analysis (TGA/DTA). The material was first heated to 110 ℃ under an atmosphere of N2 (100%) to remove free water and pre-adsorbed CO 2. Then, the mixture was heated to 1000 ℃ at a heating rate of 10 ℃ per min under a mixed atmosphere of air (40%) and N2 (60%). The ionic liquid content was 74wt% as calculated from the change in sample mass over a temperature range of 150 ℃ to 1000 ℃. The initial decomposition temperature of the ionic liquid was 378 ℃.
The ionic liquid adsorbing material adsorbs CO2 under 100kPa and 120 ℃, desorbs under 0kPa and 120 ℃, and circularly adsorbs and desorbs for 300 times, and the adsorption capacity is reduced by 2.5 percent.
Comparative examples
20g of tween80 were dissolved in 0.001M hydrochloric acid at room temperature, 10g of mesitylene and 150 mg of ammonium fluoride were added thereto, and the mixture was heated to 37 ℃ with stirring for 90 min. 30g of sodium silicate and 10g of Fe3O4 were added and heated to 120 ℃ for 24h, the mixture was cooled to room temperature, filtered to give a white solid product and dried in air and calcined at 400 ℃ for 8 h.
The adsorbing material adsorbs CO2 at 100kPa and 120 ℃, and the saturated adsorption capacity is 10.5mg/g after the equilibrium is reached.
Claims (10)
1. For CO2The trapped magnetic ionic liquid nano-composite adsorption material is characterized in that the magnetic ionic liquid nano-composite adsorption material is a composite material in which an amino group-containing ionic liquid is loaded on the surface of a nano-magnetic material carrier.
2. The method for CO of claim 12The trapped magnetic ionic liquid nano composite adsorbing material is characterized in that the content of the loaded ionic liquid is 20-90 wt%, and preferably the content of the loaded ionic liquid is 40-70 wt%; the nano magnetic material is Fe3O4-SiO2。
3. Use according to claim 1 or 2 for CO2The preparation method of the trapped magnetic ionic liquid nano composite adsorbing material is characterized by comprising the following steps of:
step 1: FeCl3.6H2O and FeCl2.4H2O is added to [ Bmim ] under nitrogen protection]Stirring and fully mixing the solution in Cl, then gradually dropwise adding concentrated ammonia water into the system for reaction, and reacting the ammonia water with reactants in the solution layer to generate Fe3O4，Fe3O4Washing, magnetically separating and drying to obtain powdered Fe3O4Particles;
step 2: dissolving surfactant in hydrochloric acid at room temperature, adjusting pH to 1-5, adding mesitylene and ammonium fluoride, heating the mixture to 37-38 deg.C under stirring, maintaining for more than 30min, and adding powdered Fe3O4Adding the granules and silicon source compound and heating to 100-1Maintaining the temperature at 20 ℃ for 20-22h, cooling the mixture to room temperature, performing magnetic separation to obtain a solid product, washing, performing magnetic separation, drying and calcining at 400-450 ℃ for more than 8 hours;
and step 3: dissolving the ionic liquid in ethanol, dispersing the carrier obtained in the step 2 in the ethanol solution of the ionic liquid, stirring for 8-10 hours at 20-50 ℃, washing, carrying out magnetic separation, drying to obtain powdery particles, removing ethanol, and drying at 50-60 ℃ to obtain the magnetic ionic liquid composite adsorbing material.
4. The method according to claim 3, wherein the cation of the ionic liquid is one or more of organic amine salt cation and organic alcohol amine cation.
5. The preparation method according to claim 3, wherein the anion of the ionic liquid is an anion having an amino acid structure, and the amino acid has a structural formula of H2N-R-COOH (R ═ CnH2n, n ═ 1-5).
6. The process according to claim 3, wherein the surfactant is a nonionic surfactant pan80, tween series; the cationic surfactant is one or more of sodium bis (2-ethylhexyl) succinate sulfonate, hexadecyl trimethyl ammonium bromide and hexadecyl trimethyl amine; the anionic surfactant is one or more of sodium lauryl sulfate.
7. The process according to claim 3, wherein the silicon source compound is ethyl silicate, sodium silicate, NaHSi2O5.3H2O, respectively.
8. The preparation method according to claim 3, wherein the mass ratio of the surfactant to the mesitylene is 2: 1-1: 4; the mass ratio of the silicon source compound to the surfactant is 3: 1-1: 3.
9. According to the rightUse according to claim 1 or 2 for CO2Application of trapped magnetic ionic liquid nano composite adsorption material, which is characterized by being suitable for CO2The partial pressure is 5kPa-1 MPa.
10. Use for CO according to claim 92Application of trapped magnetic ionic liquid nano composite adsorption material, which is characterized in that CO is adsorbed2The temperature is 30-130 ℃.
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