CN112742349A - For CO2Trapped magnetic ionic liquid nano composite adsorption material - Google Patents

For CO2Trapped magnetic ionic liquid nano composite adsorption material Download PDF

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CN112742349A
CN112742349A CN201911040672.4A CN201911040672A CN112742349A CN 112742349 A CN112742349 A CN 112742349A CN 201911040672 A CN201911040672 A CN 201911040672A CN 112742349 A CN112742349 A CN 112742349A
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ionic liquid
magnetic
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mixture
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江洋洋
陈曦
黄钟斌
孔京
汪东
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D53/00Separation 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
    • B01D53/02Separation 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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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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

For CO2Trapped magnetic ionic liquid nano composite adsorption material
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 ℃.
CN201911040672.4A 2019-10-30 2019-10-30 For CO2Trapped magnetic ionic liquid nano composite adsorption material Pending CN112742349A (en)

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