CN106984137B - CO absorption device capable of realizing rapid phase separation2Preparation and use method of polyamino acid ionic liquid type phase separation absorbent - Google Patents
CO absorption device capable of realizing rapid phase separation2Preparation and use method of polyamino acid ionic liquid type phase separation absorbent Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01D53/14—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 absorption
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Abstract
The invention provides a phase separable CO2An absorbent system. CO capture by absorbent2Will phase separate to rich CO2Solid phase of (2) and oligoCO2Of the liquid phase of (2) to only CO-rich2The solid phase is heated for desorption, thus avoiding the energy consumed by heating the solvent. Simultaneously, the polyamino acid ionic liquid and magnetic nano-ions (Fe)3O4) Recombination, CO capture2After that, phase separation still occurs. The enriched CO is generated by the action of an external magnetic field2The solid phase is rapidly settled and separated from the liquid phase, so that the time is saved, the efficiency is improved, and compared with the traditional absorbent, the absorbent still has the advantage of low regeneration energy consumption.
Description
Technical Field
The invention relates to CO2The technical field of absorption, in particular to the absorption of CO by liquid2The technical field is as follows.
Background
Along with the rapid development of global economy, diversification and regional economy integration, global climate disasters caused by climate warming enable the world to think about the traditional economic development mode again. The carbon emission generated by the traditional high-carbon economic mode characterized by high energy consumption, high pollution and high emission and the global climate change brought by the carbon emission meet the general welfare of the current and future human society, and the acceleration of the economic development mode conversion becomes the necessary trend of the global economic development. China CO in recent years2Discharge capacity of the head of the worldThe current situation of the situation makes China face public opinion pressure from international society, the existing extensive economic growth mode is not suitable for the requirement of economic development of China, the development of low-carbon economy becomes a way for changing the existing economic mode, and China starts to bring climate change coping, energy conservation and emission reduction into the national strategy.
At present, a mature and industrially widely used method for treating acidic gases is a chemical solvent absorption method, and amine compounds are commonly used as absorbents in the method. Conventional chemical absorbents are used to treat CO during recycling2The absorption is not high, the loss of the absorbent is large, the regeneration energy consumption is high, and the defects of system corrosion exist. Therefore, there is an urgent need for a highly efficient, environmentally friendly, low energy consumption, pollution-free CO2An absorbent. The phase separation absorbent is a novel gas absorption system, and can separate different phase states after reacting with gas, such as liquid-liquid two phase, solid-liquid two phase, liquid-liquid three phase and the like, thereby having value and significance of in-depth research.
At present, CO2The methods of capturing and separating mainly include solvent absorption, adsorption, membrane separation, etc., and these methods also have certain defects and limit further applications.
The chemical solvent absorption method is a mature method for treating acid gas with wide industrial application, and has the main advantages that: to CO2Good separation effect and can obtain CO with high purity2Can treat CO with very low partial pressure2And (4) mixing the gases. Of course, the method also has the defects of strong corrosion to equipment, easy foaming, high energy consumption for solvent regeneration and the like. The ionic liquid has many excellent characteristics, such as low vapor pressure, low melting point, good thermal stability, strong dissolving capacity, difficult combustion, adjustable structure and the like. However, ionic liquids with high viscosity, especially functionalized ionic liquids, absorb CO2The post-viscosity increases sharply, resulting in CO due to the decrease of mass transfer efficiency2The absorption efficiency is reduced. The viscosity of the ionic liquid can be reduced after the ionic liquid and the water are compounded, however, in the regeneration process of the absorbent, a large amount of energy is consumed due to heating of the solvent, and the regeneration energy consumption is greatly increased.
Disclosure of Invention
First, the present invention provides a phase separable CO2An absorbent system. CO capture by absorbent2Will phase separate to rich CO2Solid phase of (2) and oligoCO2Of liquid phase of (2), only for CO enrichment2The solid phase is heated for desorption, thus avoiding the energy consumed by heating the solvent.
Secondly, the invention also provides a method for preparing the polyamino acid ionic liquid and magnetic nano-ions (Fe)3O4) Recombination, CO capture2After that, phase separation still occurs. The enriched CO is generated by the action of an external magnetic field2The solid phase is rapidly settled and separated from the liquid phase, so that the time is saved, the efficiency is improved, and compared with the traditional absorbent, the absorbent still has the advantage of low regeneration energy consumption.
The absorbent has short preparation process and CO2The absorption/desorption operation is simple, and the industrial batch production and application are easy.
Absorbent of the invention on CO2The method has the advantages of strong absorption capacity, low regeneration energy consumption, environmental protection and simple operation.
The invention provides a phase separation CO absorption method2The preparation method of the polyamino acid ionic liquid comprises the following steps:
1 Synthesis of Polydimethyldiallylammonium chloride (PDADMAC)
Weighing [66.6688g, 247.41mmol]Dimethyldiallylammonium chloride solution, [0.6g,2.63mmol]Initiator ammonium persulfate (K)2S2O8)、[0.0025g,7.5×10-3mmol]Complexing agent disodium ethylene diamine tetraacetate (EDTA-2Na), [0.928g,10mmol]The chain transfer agent thioglycolic acid (TGA) was dissolved in 10mL of ultra pure water, respectively. Mixing the samples at room temperature, magnetically stirring, and introducing N2. Transferring to 70 deg.C water bath after 20min, reacting for 24 hr, heating to 80 deg.C, maintaining for 6 hr, stopping reaction, and cooling to room temperature. Concentration by rotary evaporation, followed by vacuum drying for 48 h. To obtain the poly dimethyl diallyl ammonium chloride (PDADMAC).
2 preparation of P [ DADMAC ] [ OH ] (ion exchange)
Poly (dimethyldiallylammonium chloride) (PDADMAC) was weighed out in an amount of [8.0835g, 0.05mol ], and dissolved in 40mL of ultrapure water. The washed 717 anion exchange resin was loaded into a chromatography column having a diameter of 4cm, and the height of the loaded resin was 12 cm. The resin was rinsed again with ultrapure water and after 3 times the pH of the running water was recorded until it remained unchanged. Adding PDADMAC aqueous solution, allowing the PDADMAC aqueous solution to naturally flow through the resin, and recording the pH value of the flowing solution; the solution flowing down was again poured back onto the column and the pH was recorded after natural flow down. Repeating the above operations until the pH value of the solution is unchanged, and finishing the ion exchange to obtain a P [ DADMAC ] [ OH ] solution.
3 preparing polyamino acid ionic liquid (P [ DADMAC ] [ AA ]) (neutralization reaction)
Adding [0.05mol ] into the obtained quaternary ammonium alkali aqueous solution]Amino acid or its derivative (based on the amount of-OH contained in the amino acid, the molar amount of-OH is the same as the molar amount of quaternary ammonium base). N is a radical of2And (4) performing magnetic stirring at 40 ℃ under the atmosphere, and reacting for 24 hours. Concentration by rotary evaporation, followed by vacuum drying at 60 ℃ for 48 h. And obtaining the product polyamino acid ionic liquid.
4 preparing polyamino acid ionic liquid-magnetic particle complex (PAAILs-Fe)3O4)
Preparing aqueous solution of polyamino acid ionic liquids (PAAILs), adding Fe3O4The mass ratio of the magnetic nanoparticles to the PAAILs is 0.03-1%. Shaking at constant temperature of 25 deg.C for 20 min.
The invention also provides a phase separation CO absorption method2The use method of the polyamino acid ionic liquid comprises the following steps:
1 preparing polyamino acid ionic liquids (PAAILs), and introducing CO into the PAAILs2；
2, separating the solid phase from the liquid phase obtained by phase separation by centrifugation, and taking out the solid phase;
3 will be rich in CO2Heating the solid phase to 120 ℃, keeping the temperature for 4h, taking out, and dissolving the desorbed solid phase in the original liquid phase again.
In this way, the CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
Preferably, a phase separated absorption of CO is provided2Of the polyamino acid ionic liquidThe method comprises the following steps:
1-oriented polyamino acid ionic liquid-magnetic particle complex (PAAILs-Fe)3O4) Introducing CO into the absorbent liquid2；
2, rapidly separating the solid phase and the liquid phase by an external magnetic field, and taking out the solid phase;
3 will be rich in CO2Heating the solid phase to 120 ℃, keeping the temperature for 4 hours, taking out the solid phase, and dissolving the desorbed solid phase in the original liquid phase again.
In this way, the CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
Drawings
FIG. 1 is a graph of solid phase settling time of CO2 absorbed by [ PDADMAC ] [ Gly ], [ PDADMAC ] [ Gly ] -Fe3O 4.
FIG. 2 is a graph showing the solid phase settling time of CO2 absorbed by [ PDADMAC ] [ Trp ], [ PDADMAC ] [ Trp ] -Fe3O 4.
FIG. 3 phase separation of aqueous absorbents of varying concentrations P [ DADMAC ] [ Trp ] capturing CO 2.
FIG. 4P regeneration cycling performance (absorption/desorption) profile of [ DADMAC ] [ Trp ] absorbent.
Detailed Description
Example one
1 Synthesis of Polydimethyldiallylammonium chloride (PDADMAC)
Weighing [66.6688g, 247.41mmol]Dimethyldiallylammonium chloride solution, [0.6g,2.63mmol]Initiator ammonium persulfate (K)2S2O8)、[0.0025g,7.5×10-3mmol]Complexing agent disodium ethylene diamine tetraacetate (EDTA-2Na), [0.928g,10mmol]The chain transfer agent thioglycolic acid (TGA) was dissolved in 10mL of ultra pure water, respectively. Mixing the samples at room temperature, magnetically stirring, and introducing N2. Transferring to 70 deg.C water bath after 20min, reacting for 24 hr, heating to 80 deg.C, maintaining for 6 hr, stopping reaction, and cooling to room temperature. Concentration by rotary evaporation, followed by vacuum drying for 48 h. Obtaining the product of the first step.
2 preparation of P [ DADMAC ] [ OH ] (ion exchange)
Poly (dimethyldiallylammonium chloride) (PDADMAC) was weighed out in an amount of [8.0835g, 0.05mol ], and dissolved in 40mL of ultrapure water. The washed 717 anion exchange resin was loaded into a chromatography column having a diameter of 4cm, and the height of the loaded resin was 12 cm. The resin was rinsed again with ultrapure water and after 3 times the pH of the running water was recorded until it remained unchanged. Adding PDADMAC aqueous solution, allowing the PDADMAC aqueous solution to naturally flow through the resin, and recording the pH value of the flowing solution; the solution flowing down was again poured back onto the column and the pH was recorded after natural flow down. Repeating the above operations until the pH value of the solution is unchanged, and finishing the ion exchange.
3 preparation of polyamino acid Ionic liquid-P [ DADMAC ] [ AA ] (neutralization reaction)
Adding [0.05mol ] into the obtained quaternary ammonium alkali aqueous solution]Amino acid or its derivative (based on the amount of-OH contained in the amino acid, the molar amount of-OH is the same as the molar amount of quaternary ammonium base). N is a radical of2And (4) performing magnetic stirring at 40 ℃ under the atmosphere, and reacting for 24 hours. Concentration by rotary evaporation, followed by vacuum drying at 60 ℃ for 48 h. Thus obtaining the product of polyamino acid ionic liquid (PAAILs).
4 PAAILs-Fe3O4Preparation of the absorbent
CO from aqueous 5 PAAILs absorbents2Absorption and phase separation
6 rich in CO2Desorption regeneration of solid phase
The solid phase and the liquid phase are separated by centrifugation, the solid phase is taken out, and the liquid phase is not treated. Will be rich in CO2Heating the solid phase to 120 ℃, keeping the temperature for 4h, taking out, and dissolving the desorbed solid phase in the original liquid phase again. CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
7 PAAILs-Fe3O4CO of absorbent2Absorption and phase separation
To PAAILs-Fe3O4Introducing CO into the absorbent2. Recording CO introduction2The mass before and after and the pH value, and phase separation was observed. And (3) rapidly separating the solid phase from the liquid phase separated by the external magnetic field, and taking out the solid phase without any treatment on the liquid phase. Will be rich in CO2Heating the solid phase to 120 ℃, keeping the temperature for 4 hours, taking out the solid phase, and dissolving the desorbed solid phase in the original liquid phase again. CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
Example two
1 polyglycine ionic liquid P [ DADMAC ]][Gly]CO of aqueous absorbent2Absorption and phase separation
Preparing 3mol/L P [ DADMAC ]][Gly]Taking 6mL of absorbent as aqueous solution, and introducing CO into the aqueous solution2. Recording CO introduction2The mass before and after and the pH value, and phase separation was observed.
2 rich in CO2Desorption regeneration of solid phase
The solid phase and the liquid phase are separated by centrifugation, the solid phase is taken out, and the liquid phase is not treated. Heating the solid phase to 120 ℃, keeping the temperature for 4h, taking out, and dissolving the desorbed solid phase in the original liquid phase again. CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
3 P[DADMAC][Gly]-Fe3O4Preparation of the absorbent
Preparing 3mol/L P [ DADMAC ]][Gly]Taking 6mL of absorbent as an aqueous solution, and adding 1mg of Fe3O4Nanoparticles. Shaking at constant temperature of 25 deg.C for 20 min. And testing the hydrated particle size and the Zeta potential of the absorbent to determine the compounding condition.
4 P[DADMAC][Gly]-Fe3O4CO of absorbent2Absorption and phase separation
Introducing CO into the absorbent2. Recording CO introduction2The mass before and after and the pH value, and phase separation was observed.
5 rich in CO2Desorption regeneration of solid phase
The solid phase and the liquid phase which are separated are rapidly separated by an external magnetic field,the solid phase is taken out and the liquid phase is not treated. Heating the solid phase to 120 ℃, keeping the temperature for 4h, taking out, and dissolving the desorbed solid phase in the original liquid phase again. CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
Example three
1 polytryptophane ionic liquid P [ DADMAC ]][Trp]CO of aqueous absorbent2Absorption and phase separation
Preparing 0.5mol/L P [ DADMAC ]][Trp]Taking 6mL of absorbent as aqueous solution, and introducing CO into the aqueous solution2. Recording CO introduction2The mass before and after and the pH value, and phase separation was observed.
2 rich in CO2Desorption regeneration of solid phase
The solid phase and the liquid phase are separated by centrifugation, the solid phase is taken out, and the liquid phase is not treated. Heating the solid phase to 120 ℃, keeping the temperature for 4h, taking out, and dissolving the desorbed solid phase in the original liquid phase again. CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
3 P[DADMAC][Trp]-Fe3O4Preparation of the absorbent
Preparing 0.5mol/L P [ DADMAC ]][Trp]Taking 6mL of absorbent as an aqueous solution, and adding 2mg of Fe3O4Nanoparticles. Shaking at constant temperature of 25 deg.C for 20 min. And testing the hydrated particle size and the Zeta potential of the absorbent to determine the compounding condition.
4 P[DADMAC][Trp]-Fe3O4CO of absorbent2Absorption and phase separation
Introducing CO into the absorbent2. Recording CO introduction2The mass before and after and the pH value, and phase separation was observed.
5 rich in CO2Desorption regeneration of solid phase
And (3) rapidly separating the solid phase from the liquid phase separated by the external magnetic field, and taking out the solid phase without any treatment on the liquid phase. Heating the solid phase to 120 ℃, keeping the temperature for 4h, taking out, and dissolving the desorbed solid phase in the original liquid phase again. CO is carried out again2Absorption, solid phase separation, desorption and regeneration. And (6) circulating.
P[DADMAC][Gly]-Fe3O4Granule of (1)Radial and Zeta potential table
P[DADMAC][Trp]-Fe3O4Particle diameter and Zeta potential table
[PDADMAC][Gly]And [ PDADMAC ]][Gly]-Fe3O4Table of CO2 absorption capacity
[PDADMAC][Gly](3mol/L) absorption of CO2After solid phase settling time table
[PDADMAC][Gly]-Fe3O4Absorption of CO2After solid phase settling time table
[PDADMAC][Trp]CO of2Absorption capacity meter
[PDADMAC][Trp]Absorption of CO2After solid phase settling time table
[PDADMAC][Trp]-Fe3O4(0.2%) absorption of CO2After solid phase settling time table
[PDADMAC][Trp]-Fe3O4(0.1%) absorption of CO2After solid phase settling time table
P[DADMAC][Gly]CO of2Absorption capacity and phase separation table
Claims (3)
1. CO absorption device capable of realizing rapid phase separation2The preparation method of the polyamino acid ionic liquid phase separation absorbent is characterized in that:
synthesis of Polydimethyldiallylammonium chloride 66.6688g, 247.41mmol of dimethyldiallylammonium chloride solution, 0.6g,2.63mmol of initiator ammonium persulfate, 0.0025g,7.5 × 10-3Respectively dissolving disodium ethylene diamine tetraacetate serving as a complexing agent and thioglycolic acid serving as a chain transfer agent of 0.928g and 10mmol in 10mL of ultrapure water;
mixing the samples at room temperature, magnetically stirring, and introducing N2；
Transferring to a 70 ℃ water bath after 20min, reacting for 24h, heating to 80 ℃, maintaining for 6h, and stopping reaction;
preparing aqueous solution of quaternary ammonium base;
preparing polyamino acid ionic liquid;
preparing a polyamino acid ionic liquid-magnetic particle compound, wherein the mass ratio of the magnetic particles to the polyamino acid ionic liquid is 0.03-1%;
the preparation of the aqueous quaternary ammonium base solution: 8.0835g of poly dimethyl diallyl ammonium chloride of 0.05mol are weighed and added into 40mL of ultrapure water for dissolution;
adding the washed 717 anion exchange resin into a chromatographic column with the diameter of 4cm, wherein the height of the added resin is 12 cm; cleaning the resin with ultrapure water, and recording the pH value of the flowing water after 3 times until the pH value is kept unchanged;
adding a poly dimethyl diallyl ammonium chloride aqueous solution, allowing the poly dimethyl diallyl ammonium chloride aqueous solution to naturally flow through the resin, and recording the pH value of the solution flowing downwards; pouring the flowing solution back to the chromatographic column again, and recording the pH value after the flowing solution naturally flows down; repeating the above operations until the pH value of the solution is unchanged;
the preparation of the polyamino acid ionic liquid comprises the following steps: adding 0.05mol of amino acid, N to the quaternary ammonium alkali aqueous solution2Performing magnetic stirring at 40 ℃ in an atmosphere, and reacting for 24 hours;
the preparation method of the polyamino acid ionic liquid-magnetic particle compound comprises the following steps: prepared at 1/10c concentrationSaturation ofTo cSaturation ofThe polyamino acid ionic liquid water solution is added with proper amount of Fe according to the mass ratio of 0.03-1 percent of the magnetic nano particles to the polyamino acid ionic liquid3O4Vibrating the nano particles at constant temperature of 5 ℃ for 20 min;
c is mentionedSaturation ofRefers to the saturation concentration, said 1/10cSaturation ofMeans one tenth of the saturation concentration.
2. A use method of polyamino acid ionic liquid is characterized in that:
introducing CO into the polyamino acid ionic liquid2；
Separating the solid phase from the liquid phase by centrifugation, and taking out the solid phase;
will be rich in CO2Heating the solid phase to 120 ℃, keeping the temperature for 4h, taking out, and dissolving the desorbed solid phase in the stock solution phase again;
the polyamino acid ionic liquid is prepared by the following steps:
synthesis of Polydimethyldiallylammonium chloride 66.6688g, 247.41mmol of dimethyldiallylammonium chloride solution, 0.6g,2.63mmol of initiator ammonium persulfate, 0.0025g,7.5 × 10-3mmol complexing agent disodium ethylene diamine tetraacetate, 0.928g,10mmol chain transferDissolving thioglycollic acid serving as a transfer agent in 10mL of ultrapure water respectively;
mixing the samples at room temperature, magnetically stirring, and introducing N2；
Transferring to a 70 ℃ water bath after 20min, reacting for 24h, heating to 80 ℃, maintaining for 6h, and stopping reaction;
preparation of aqueous quaternary ammonium base solution: 8.0835g of poly dimethyl diallyl ammonium chloride of 0.05mol are weighed and added into 40mL of ultrapure water for dissolution;
adding the washed 717 anion exchange resin into a chromatographic column with the diameter of 4cm, wherein the height of the added resin is 12 cm; cleaning the resin with ultrapure water, and recording the pH value of the flowing water after 3 times until the pH value is kept unchanged;
adding a poly dimethyl diallyl ammonium chloride aqueous solution, allowing the poly dimethyl diallyl ammonium chloride aqueous solution to naturally flow through the resin, and recording the pH value of the solution flowing downwards; pouring the flowing solution back to the chromatographic column again, and recording the pH value after the flowing solution naturally flows down; repeating the above operations until the pH value of the solution is unchanged;
preparing a polyamino acid ionic liquid: adding 0.05mol of amino acid, N to the quaternary ammonium alkali aqueous solution2And (4) performing magnetic stirring at 40 ℃ under the atmosphere, and reacting for 24 hours.
3. A rapidly phase-separable CO-absorbing material prepared by the method of claim 12The use method of the polyamino acid ionic liquid phase separation absorbent is characterized in that:
introducing CO into absorbent liquid of polyamino acid ionic liquid-magnetic particle composite2；
Rapidly separating the solid phase and the liquid phase by an external magnetic field, and taking out the solid phase;
will be rich in CO2Heating the solid phase to 120 ℃, keeping the temperature for 4 hours, taking out the solid phase, and dissolving the desorbed solid phase in the original liquid phase again.
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